Abstract:
1,2-Unsaturated carboxylic acids having carbonyl compound impurities are separated by binding the carbonyl compounds with inorganic, aliphatic or aromatic amines and then distilling the acids.
Abstract:
Lower alkyl mercaptans prepared from alkanols and hydrogen sulfide are obtained in pure form by separating the gaseous mixture of hydrogen sulfide, alkanol, alkyl mercaptan, dialkyl sulfide, water, dialkyl either and inert gases at a pressure up to 10 atm. (gauge) and a temperature of 10* to 140* C. into volatile and non-volatile portions, the volatiles washed countercurrently to remove entrained alkyl mercaptan and after separating of the volatile hydrogen sulfide and ethers from the mercaptan the mercaptan is further separated from the other nonvolatiles as a substantially pure product.
Abstract:
Suspension or solutions of cyanuric chloride in water containing organic solvents are prepared at high mixing velocities and low temperatures with resulting low degree of hydrolysis by introducing liquid cyanuric chloride through a nozzle in the upper portion of the mixing apparatus in countercurrent flow to upwardly flowing solvent introduced from at least one lower nozzle above a breast shaped constriction in the lower, open portion of the apparatus. In this way the chamber walls are always covered with an unbroken layer of liquid. The process can be carried out at normal, reduced or elevated pressure. At reduced pressure by evaporation of the solvent there is simultaneously a cooling of the system.
Abstract:
Process for continuous production of propylene oxide (FIG. 1) from propylene and aqueous hydrogen peroxide. The aqueous hydrogen peroxide is first reacted with propionic acid in the presence of acid catalyst to form perpropionic acid (1). The perpropionic acid is taken up by extraction in benzene (5 , 12), and following drying of the benzene solution (16), the perpropionic acid in the solution is reacted with propylene (18) for oxidation of the propylene to propylene oxide and conversion of the perpropionic acid back to propionic acid. The reaction mixture is worked up to separate propylene oxide, propionic acid and benzene (25, 27, 31, 33), and the latter two are recycled. In the benzene extraction (5, 12), an aqueous raffinate (7) is formed containing hydrogen peroxide and acid catalyst. Water is removed from the aqueous raffinate (8) and the concentrate is recycled to the propionic acid reactor. Make-up hydrogen peroxide can be added to the aqueous raffinate before the removal of water.
Abstract:
The residual gases obtained in the production of cyanuric chloride having a pressure of 1-5 bar (absolute) preferably 1-4 bar, are worked up by leading them into the lower portion of a column, reacted in the column with at least the equivalent amount of hydrogen cyanide to form cyanogen chloride and led in countercurrent flow to the water charged to the upper portion of the column whereupon the aqueous solution of cyanogen chloride formed is withdrawn from the lower portion of the column and preferably is returned into the production portion of the plant for recovery of the cyanogen chloride while the purified waste gas of the column leaves in the upper portion of the column.
Abstract:
There is provided a process for the production of a solution or suspension of cyanuric chloride in a water containing organic solvent wherein the liquid cyanuric chloride and the organic-aqueous solvent are mixed together while being agitated, the liquid cyanuric chloride at a temperature between its melting point and 200 DEG C. is led into the flowing organic-aqueous solvent with a velocity of Vcy (in kg per hour) wherein where P is the desired concentration of cyanuric chloride in the solution or suspension to be produced in weight %, PLM is the concentration of cyanuric chloride in the solvent used which also includes O, VLM is the velocity of the solvent added in kg/h, AND PLM, VLM and TLM, the temperature of the added solvent, are so selected that the expression does not exceed the boiling temperature in DEG C. of the solvent used and wherein Cp(LM) and Cp(Cy) signify the specific heat capacities in cal. x g 1 x ( DEG degree C) 1 of the solvent and cyanuric chloride respectively, whereupon in a given case within at most 3 minutes after bringing the cyanuric chloride and solvent into contact the flowing mixture is cooled to the desired storage temperature.
Abstract:
There is provided a process, preferably continuous and in a given case successive, substitution of one or two chlorine atoms of cyanuric chloride by one or two amines, which may be the same or different, in the presence of an acid acceptor and in the presence of an organic solvent, particularly for the production of 2-alkylamino-4,6-dichloro and preferably for the production of 2,4-di(alkylamino)-6-chloro-s-triazines wherein there is added 1.00 to 1.05 mole, preferably 1.00 to 1.03 mole of a first amine to a 4.5 to 50 weight % suspension or solution of cyanuric chloride in a mixture of 65 to 85 weight % of xylene, toluene, ethylbenzene, benzene and/or an aliphatic or cycloaliphatic hydrocarbon with 5 to 10 carbon atoms (toluene being preferred) and 35 to 15 weight % of a ketone with 3 to 8 carbon atoms, preferably acetone, while maintaining the temperature between about 0 and about 20 DEG C, preferably about 10 to 18 DEG C., continuously so regulating the pH value of the reaction mixture obtained in accordance with the reaction time by addition of alkali and in a given case, water so that this corresponds to a point within the area bounded by lines ABCD of FIG. 1, which runs through the area beginning with the reaction time t,(step 1)= 0 until reaching a position in the area bounded by the lines BCEF and after reaching a pH of 7.0, preferably 7.2 maintains a temperature of about 10 DEG to about 60 DEG C., preferably about 25 DEG to 40 DEG C., after addition of 0.96 to 1.05, preferably 0.98 to 1.02 equivalents of alkali per mole of cyanuric chloride, adding at least an equimolar amount, preferably 1.00 to 1.02 mole of the second amine per mole of cyanuric chloride and continuously so adjusting the pH value of the reaction mixture obtained depending on the reaction time by addition of alkali that this corresponds to a point within the area which is defined by lines GHIJ in FIG. 3 which passes through the band beginning with the reaction time t(step 2)= 0 of the second reaction step until reaching a position in the area bounded by the lines HIKL and thereby maintaining a temperature of 40 to 70 DEG C., preferably 45 DEG to 55 DEG C. and thereafter working up the product in known manner wherein t1 is a time of 4 to 10 hours, preferably about 7 hours and t2 is a time of 2 to 8 hours, preferably about 6 hours and wherein the B C corresponds to the equation, pH = -(12.6/t1)+ 14.35 and the line H I corresponds to the equation pH = -(24,857/t2)+ 23.9285. There are also disclosed novel, purified mono and bis alkylamino-cyanoalkylalkylamino - s - triazines.
Abstract:
There is provided an apparatus for bringing into contact liquids at least one of which is viscous, the apparatus consisting essentially of a tubular container, a first nozzle from introducing a liquid in the upper portion of the container, at least one other nozzle lower than the first nozzle for introducing a different liquid, the tubular container being closeable at the tap thereof and downward from said other nozzle being constricted breast shaped to form a discharge opening, said other nozzles are preferably of polished steel, said other nozzles consist essentially of at least one tangential spray means arranged in at least one row, said other nozzles being slightly above said constriction and being directed in the direction of the upper closeable device or said first nozzle and wherein the discharge opening can discharge into another container which is permanently or detachably connected to the tubular container, said further container can be provided with means for establishing reduced pressure or superatmospheric pressure.