Abstract:
High purity 4,6-dinitro-1,3-benzenediol is prepared by (a) contacting a 1,2,3-trihalobenzene with a nitrating agent and an acid under reaction conditions such that a 1,2,3-trihalo-4,6-dinitrobenzene is produced, (b) contacting the 1,2,3-trihalo-4,6-dinitrobenzene prepared in (a) with an alkanol and a base under reaction conditions such that a 4,6-dinitro-2-halo-1,3-benzenediol is produced, and (c) contacting the 4,6-dinitro-2-halo-1,3-benzenediol prepared in (b) with a hydrogenating agent in the presence of a solvent and a catalyst under reaction conditions such that a 4,6-diamino-1,3-benzenediol is produced. This 4,6-diamino-1,3-benzenediol is useful in the preparation of high molecular weight polybenzoxazoles.
Abstract:
Catalysts comprising the adduct of a Group 4b-Group 3b metal oxide composition represented by the empirical formula:(M.sup.1.sub.a M.sup.2.sub.b O.sub.c).sub.x (NO.sub.2).sub.ywherein M.sup.1 is at least one element selected from Group 4b of the Periodic Table of the Elements, M.sup.2 is at least one element selected from Group 3b of the Periodic Table of the Elements, a is 1, b is 0.05 to 20, c is a number taken to satisfy the average valences of M.sup.1 and M.sup.2 in the oxidation states in which they exist in the composition, x is 1, and y is 0 to c, and a catalytically effective amount of sulfur trioxide are useful to catalyze the nitration of aromatic compounds in the vapor phase to produce nitroaromatic compounds. The catalysts are particularly effective to catalyze the vapor phase nitration of chlorobenzene and are characterized in such reaction by providing a para/ortho isomer distribution ratio of at least about 2/1.
Abstract:
Substituted phenols are nitrated by contacting same with a 10 to 70% by weight concentrated aqueous solution of nitric acid. The subject nitration process is well adopted for the preparation, e.g., of 2,6-dichloro-4-nitrophenol, a valuable intermediate in the production of various agrochemicals/pharmaceuticals.
Abstract:
A process for the management of by-product tetranitromethane (TNM) which avoids the hazards of the prior art isolation or extraction procedures. A selected in-plant liquid or vapor stream, or a reactor off-gas stream from nitration or nitric acid oxidation plant, which contains TNM, is heated to effectively pyrolyze the TNM without undue losses of nitric acid values.
Abstract:
Aromatic compounds are nitrated in the vapor phase via a process comprising contacting the aromatic compounds with a nitrating agent in the presence of a nitration promoting catalyst comprising the adduct of a Group 4b-Group 3b metal oxide composition represented by the empirical formula:(M.sup.1.sub.a M.sup.2.sub.b O.sub.c).sub.x (NO.sub.2).sub.ywherein M.sup.1 is at least one element selected from Group 4b of the Periodic Table of the Elements, M.sup.2 is at least one element selected from Group 3b of the Periodic Table of the Elements, a is 1, b is 0 to 20, c is a number taken to satisfy the average valences of M.sup.1 and M.sup.2 in the oxidation states in which they exist in the composition, x is 1, and y is 0 to c, and a catalytically effective amount of sulfur trioxide. Such catalysts are particularly effective to catalyze the vapor phase nitration of chlorobenzene and are characterized in such reaction by providing a para/ortho isomer distribution ratio of at least about 2/1.
Abstract:
A reactor for nitration of saturated hydrocarbons having less than five con atoms, alone or in admixture, in the gaseous phase under pressure is made up of a reaction enclosure, in which a tube or pipe bank is in contact with a heated fluid of high heat-exchange capacity. The inside perimeter of the tubes does not exceed 800 mm, and if circular not in excess of 250 mm, and the ratio of the surface of the tube bank, in contact with the reaction medium, to the volume of the reaction enclosure is 1:1 to 3:1.The reactor apparatus further includes a mechanical means to uniformly distribute the delivery of reaction medium gases to the various tubes of the bank so that the load difference between the most loaded tube and that of the least loaded tube is equal to 10% at the most.The reactor also includes a tube bank injector which feeds the tube bank to assure homogeneous mixing of all the reaction fluids in the tube bank.
Abstract:
There is disclosed a method for preparing an ester of nitroacetic acid which comprises;(1) a first step of subjecting a vinyl ester of a fatty acid and a nitrogen oxide to reaction with each other in the presence of a gas containing molecular oxygen in a solvent; and(2) a second step of subjecting the resultant reaction product of the first step to reaction with an alcohol.According to the method of this invention, an ester of nitroacetic acid can effectively be obtained in higher yield.
Abstract:
Aromatic hydrocarbons are nitrated by reacting the aromatic hydrocarbon in a nitrogen tetroxide-containing liquid reaction medium, in the presence of a beta-dicarbonyl compound having a "W" configuration with a carbonyl group at each apex of the "W", such as a metal acetylacetonate, preferably at a pressure and temperature sufficient to maintain the nitrogen tetroxide in the liquid state. Addition of an inert organic co-solvent to the liquid nitrogen tetroxide for the metal acetylacetonate promoted nitration of benzene essentially eliminates the production of dinitrobenzenes.
Abstract:
Aromatic compounds are nitrated in the vapor phase via a process comprising contacting the aromatic compound with a nitrating agent in the presence of a nitration promotion catalyst which comprises the adduct of:(a) an alumina-silica-metal oxide combination represented by the formula:(Al.sub.2 O.sub.3).sub.a (SiO.sub.2).sub.b (M.sub.2/n O).sub.c wherein M is a metal cation selected from the group consisting of the lanthanides or rare earths, Groups 1b, 2b, 5b, 6b, 7b, and 8 of the Periodic Table of the Elements, and mixtures thereof, and a, b, and c represent weight percent of the Al.sub.2 O.sub.3, SiO.sub.2, and M.sub.2/n O components, respectively, in the alumina-silica-metal oxide combination, with a being 0 to 100, b being 0 to 100, and c being 0 to 50, and n represents an integer from 1 to 7 of the valence of the metal cation, with the proviso that the sum of (a+b) must be greater than 0, and(b) a catalytically effective amount of sulfur trioxide.
Abstract:
Catalyst compositions are prepared by contacting an alumina-silica-metal oxide combination represented by the formula:(Al.sub.2 O.sub.3).sub.a (SiO.sub.2).sub.b (M.sub.2/n O).sub.cwherein M is a metal cation selected from the group consisting of the lanthanides of rare earths, Groups 1b, 2b, 5b, 6b, 7b, and 8 of the Periodic Table of the Elements, and mixtures thereof, and a, b, and c represent weight percent of the Al.sub.2 O.sub.3, SiO.sub.2, M.sub.2/n O components, respectively, in the alumina-silica-metal oxide combination, with a being 0 to 100, b being O to 100, and c being 0 to 50, and n represents an integer from 1 to 7 of the valence of the metal cation, with the proviso that the sum of a+b) must be greater than 0, with a catalytically effective amount of sulfur trioxide.
Abstract translation:催化剂组合物通过使由式(Al 2 O 3)a(SiO 2)b(M2 / nO)c表示的氧化铝 - 二氧化硅 - 金属氧化物组合物接触来制备:其中M是选自稀土镧系元素的金属阳离子 元素周期表第1b,2b,5b,6b,7b和8族及其混合物,a,b和c分别表示Al 2 O 3,SiO 2,M 2 / NO组分的重量百分数, 氧化铝 - 二氧化硅 - 金属氧化物组合,其为0〜100,b为0〜100,c为0〜50,n表示金属阳离子的价数的1〜7的整数,条件是 a + b)的总和必须大于0,具有催化有效量的三氧化硫。