摘要:
A process for the preparation of acetic acid esters CH.sub.3 --CO--O--R.sup.1 (I, R.sup.1 =an organic radical other than methyl and ethyl) by alkali-catalyzed trans-esterification of an acetic acid ester CH.sub.3 --CO--O--R.sup.2 (II, R.sup.2 =methyl or ethyl) with an alcohol R.sup.1 --OH (III), accompanied by elimination of the alcohol R.sup.2 --OH (IV), wherein(a) the trans-esterification reaction is carried out in the middle section K.sub.M of a distillation column K, the alcohol III being fed as liquid into the upper zone and the ester II into the lower zone of K.sub.M,(b) the alkaline catalyst is introduced into the upper part K.sub.U of K,(c) the alcohol IV, or a mixture of IV and the ester II, is taken off the top of the column,(d) the mixture obtained from (c) (unless the alcohol IV alone is obtained) is separated in the column section K.sub.U or in a stripper column K.sub.S into IV and the azeotrope of II and IV, and the latter is recycled to the lower zone of K.sub.M,(e) the ester I is taken as vapor or liquid from the lower zone of the lower section K.sub.L of K and(f) the catalyst is either removed, or recycled to K.sub.U, in a conventional manner.
摘要:
Formamide is prepared continuously from methyl formate and ammonia, pure methanol being recovered, by a process wherein(a) the reaction of methyl formate and ammonia is carried out predominantly in the liquid phase in the upper region of a reaction column R having a total of from 15 to 30 theoretical plates,(b) the methanol formed in this reaction is removed, together with small amounts of formamide, from the column or the evaporator in vaporus form at the level of plates 1-5 (counted from the bottom),(c) the formamide is removed from this methanol/formamide mixture, together with small amounts of methanol, in a distillation column D1 and recycled to R, and(d) the small amounts of methanol contained in the bottom product from R, which substantially consists of formamide and in this column should be at from 110.degree. to 130.degree. C., are separated off in a distillation column D2.
摘要:
A process for the production of anhydrous or substantially anhydrous formic acid by hydrolysis of methyl formate which is carried out in a column having an upper fractionating section, a middle hydrolysis section and a lower extraction section and in which(a) the hydrolysis is carried out in the middle section of the columm, with water and methyl formate in countercurrent,(b) the resulting formic acid is extracted, in the lower section of the column, by means of a carboxylic acid amide which is fed into the lower end of the middle section of the column,(c) the extract phase, consisting in the main of formic acid and the carboxylic acid amide, is distillatively dehydrated, or substantially dehydrated, in the lower section of the column,(d) the methanol and uncovered methyl formate are removed by fractional distillation in the upper section of the column and(e) the pure formic acid or concentrated aqueous formic acid is distilled from the anhydrous or substantially anhydrous extract phase in a second column, leaving the carboxylic acid amide.
摘要:
Formic acid is recovered, by distillation, from its mixtures with solvents of the general formula I ##STR1## where R.sup.1 is hydrogen, methyl, ethyl or vinyl and R.sup.2 and R.sup.3 are each alkyl, cycloalkyl, aryl or aralkyl, or R.sup.2 and R.sup.3 together form a 1,4- or 1,5-alkylene group, in each case of not more than 8 carbon atoms, with the provisos that the sum of the number of carbon atoms in R.sup.2 and R.sup.3 is 7 to 14 and that only one of these radicals is aryl, by a method in which the distillation is carried out in the presence of a carboxamide II which is selected from the group consisting of formamide, acetamide, propionamide and the same compounds substituted by N-methyl or N,N-dimethyl, and which has a boiling point lower than that of the solvent I.
摘要:
Anhydrous or substantially anhydrous formic acid is obtained by hydrolysis of methyl formate, in a process wherein(a) methyl formate is hydrolyzed,(b) the methanol and excess methyl formate are distilled from the hydrolysis mixture obtained,(c) the bottom product of distillation (b), consisting of formic acid and water, is extracted, in a liquid-liquid extraction, with an extractant which in the main takes up the formic acid,(d) the resulting extract phase, consisting of formic acid, the extractant and a part of the water, is subjected to distillation,(e) the top product obtained from this distillation and consisting of all or part of the water introduced into the distillation, and part of the formic acid, is recycled, as vapor, into the lower part of the distillation column of stage (b),(f) the bottom product of distillation stage (d), consisting of the extractant, with or without part of the water, and the greater part of the formic acid, is separated by distillation into anhydrous or substantially anhydrous formic acid and the extractant, and(g) the extractant leaving stage (f) is recycled to the process.
摘要:
Dimethyl carbonate is obtained pure, from its solutions in methanol, by extractive distillation carried out with a temperature of from 60.degree. C. at the top to 250.degree. C. at the bottom of the column and employing, as the extractant, an aprotic organic liquid which is substantially inert toward dimethyl carbonate, boils at above 100.degree. C. at standard pressure, is miscible with dimethyl carbonate in all proportions and has a dielectric constant .epsilon. of from 4 to 90 and a dipole moment .mu. of from 1.5 to 5 Debye.
摘要:
Apparatus and processes for continuous distillative separation of a mixture comprising one or more alkanolamine(s) are described. The separation is performed in one or more dividing wall column(s) and the alkanolamine or the alkanolamines is/are withdrawn as a side draw stream or side draw streams (side fraction(s)).
摘要:
What is described is a process for obtaining maleic anhydride by distillation from a solution of maleic anhydride in a high-boiling absorbent which has been obtained by gas phase oxidation of a hydrocarbon and at least partial absorption of the oxidation products into the absorbent, by i) introducing the solution into the side of a feed column with a rectifying section disposed above the feed point and a stripping section disposed below the feed point, ii) providing an upper combining column which communicates with the upper end of the rectifying section and a lower combining column which communicates with the lower end of the stripping section, iii) providing a draw column which communicates with the upper combining column and the lower combining column, iv) drawing maleic anhydride off as a side draw from the draw column, and drawing off compounds having a lower boiling point than maleic anhydride at the top of the upper combining column and the high-boiling absorbent at the bottom of the lower combining column. The maleic anhydride obtained as a side draw has a low content of acrylic acid and acetic acid.
摘要:
A process is described for continuously hydrogenating unsaturated compounds, in which particles of a first hydrogenation catalyst are suspended in a liquid phase in which an unsaturated compound is dissolved, the liquid phase, in the presence of a hydrogenous gas at a first partial hydrogen pressure and at a first temperature, is conducted through a packed bubble column reactor in cocurrent counter to the direction of gravity, the effluent from the bubble column reactor is sent to a gas-liquid separation, the liquid phase is sent to a crossfiltration to obtain a retentate and a filtrate, the retentate is recycled into the bubble column reactor and the filtrate, in the presence of a hydrogenous gas at a second partial hydrogen pressure and at a second temperature, is passed over a bed of a second hydrogenation catalyst, wherein the second partial hydrogen pressure is at least 10 bar higher than the first partial hydrogen pressure.
摘要:
The present invention provides a process for preventing fumaric acid deposits in the preparation of maleic anhydride, comprising the following steps:a) absorption of a C4-dicarboxylic acid or of a derivative from a crude product mixture into an organic solvent or water as an absorbent,b) removal of the C4-dicarboxylic acid or of a derivative from the absorbent,the absorbent thus recovered being catalytically hydrogenated fully or partly and recycled fully or partly into the absorption stage (a).