摘要:
A process for the preparation of .epsilon.-caprolactone comprising:(a) reacting cyclohexanone with a solution of perpropionic acid in an organic solvent at a molar ratio of cyclohexanone;perpropionic acid of about 1.1-5:1 at a temperature of about 10.degree. to 80.degree. C. to form a reaction mixture consisting essentially of .epsilon.-caprolactone, propionic acid and organic solvent,(b) distilling the reaction mixture from (a) in a first distillation unit to obtain a distillate comprising the organic solvent and a distillation residue,(c) introducing the distillation residue from (b) at a point into a second distillation unit to obtain a distillate comprising propionic acid and unreacted cyclohexanone, removing from the second distillation unit, separately from one another and at a point below the point of introduction into the second distillation unit, .epsilon.-caprolactone and any high-boiling constituents, and,(d) distilling in a third distillation unit the distillate from (c) to obtain a distillate consisting essentially of propionic acid and a distillation residue comprising a mixture of propionic acid and cyclohexanone.
摘要:
Very pure carboxylic acid-1-monoglycerides are prepared by reacting a carboxylic acid with glycidol at a temperature of 80.degree. to 200.degree. C. in the presence of a basic alkali metal or alkaline earth metal compound as a catalyst in the presence of an inert solvent which forms a homogeneous solution with the reactants at the reaction temperature.
摘要:
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.degree. C. is led into the flowing organic-aqueous solvent with a velocity of Vcy (in kg per hour) wherein ##EQU1## where P is the desired concentration of cyanuric chloride in the solution or suspension to be produced in weight %, P.sub.LM is the concentration of cyanuric chloride in the solvent used which also includes O,V.sub.lm is the velocity of the solvent added in kg/h,And P.sub.LM, V.sub.LM and T.sub.LM, the temperature of the added solvent, are so selected that the expression ##EQU2## does not exceed the boiling temperature in .degree. C. of the solvent used and wherein C.sub.p (LM) and C.sub.p (Cy) signify the specific heat capacities in cal. x g.sup.-.sup.1 .times. (.degree.degree C).sup.-.sup.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.
摘要:
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.
摘要:
In order to be independent of the situation in regard to methane and natural gas and at the same time to obtain a heating gas there is employed in the hydrocyanic acid-methane-ammonia process (the BMA process) in place of methane an alkanol or alkanediol having 2-4 carbon atoms, preferably ethyl alcohol, and this is reacted with ammonia in a C:N ratio of 0.8:1 to 2:1. Optionally additional hydrogen can be present.
摘要:
Process for isolating propylene glycol diacarboxylates in the preparation of propylene oxide by reaction of propylene with a solution of percarboxylic acid in an organic solvent, the boiling point of which is lower than that of the carboxylic acid which corresponds to the percarboxylic acid used as the epoxidizing agent, and higher than that of propylene oxide, separation, by distillation, of the reaction mixture which essentially contains propylene oxide, the carboxylic acid corresponding to the percarboxylic acid used as the epoxidizing agent and one or more of the by-products propyleneglycol, propylene glycol monocarboxylate and propylene glycol dicarboxylate as well as propylene and the organic solvent, into a fraction containing propylene oxide and propylene and a fraction containing the carboxylic acid, the by-products mentioned and the organic solvent and further separation of the fractions into the individual components by distillation. The fraction containing the carboxylic acid, one or more of the by-products propylene glycol, propylene glycol monocarboxylate and propylene glycol dicarboxylate, and the organic solvent is distilled in a column at pressures of 1.5 to 6 bars and with an average residence time of 10 to 90 minutes in the sump. The organic solvent is removed as the top product and the carboxylic acid and the corresponding propylene glycol dicarboxylate is obtained as the sump product. From the sump product the propylene glycol dicarboxylate is isolated in a manner which is in itself known.
摘要:
Penicillamine or a homolog thereof is obtained by reacting a 2-disubstituted-5,5-alkyl-thiazolidine nitrile, alkyl having 1 to 6 carbon atoms, with a mineral acid in a two-stage proceeding wherein in the first stage relatively low temperatures and a relatively high concentration of the mineral acid are employed while in the second stage the concentration of the acid is relatively low and the temperatures are relatively high, the term "relatively" referring to the relationship of said two stages of the reaction with mineral acid.
摘要:
Pure racemic acid (dl-tartaric acid) and meso tartaric acid are produced by reaction of an alkali maleate with aqueous hydrogen peroxide in the presence of a catalyst which is an alkali molybdate or a mixture of an alkali molybdate and alkali tungstate in a process wherein the molar ratio of hydrogen peroxide to maleic acid is greater than 1:1 and the alkali salt of cis-epoxysuccinic acid formed together with the catalyst in a given case after destroying the excess hydrogen peroxide and other peroxygen compounds, are converted to free cis-epoxysuccinic acid and free molybdic acid or mixture of free molybdic acid and free tungstic acid by leading them over a strongly acidic cation exchanger, whereupon the hydrolysis of the free cis-epoxysuccinic acid to racemic acid and meso-tartaric acid can take place either in the presence of or the absence of the free molybdic acid or mixture of free molybdic acid and free tungstic acid, whereby the catalyst in the case of catalyst free hydrolysis before, and in the case of catalyst containing hydrolysis after this hydrolysis is removed with an anion exchanger and the racemic acid is then in known manner crystallized out of the catalyst free hydrolysis mixture by lowering the temperature in a given case with evaporation of water, whereupon the meso-tartaric acid remains in the mother liquor, and there is recovered from the mother liquor either by crystallization or by evaporation to dryness, in a given case in admixture with racemic acid, unreacted cis-epoxysuccinic acid and maleic acid, while the anion exchanger laden with the molybdic acid or mixture of molybdic acid and tungstic acid is regenerated in known manner with dilute aqueous alkali and, in a given case, the resulting solution of alkali molybdate or mixture of alkali molybdate and alkali tungstate, eventually after treatment with activated carbon is returned directly into the epoxidation step.
摘要:
Cyanogen chloride or cyanogen bromide is prepared by reaction of hydrogen cyanide with hydrogen chloride or hydrochloric acid (or hydrogen bromide or hydrobromic acid) and hydrogen peroxide in aqueous medium in the presence of cupric and ferric ions under superatmospheric pressure, preferably between 1.5 and 16 bar, and the cyanogen chloride (or cyanogen bromide) recovered separated from oxygen and nitrogen. In a preferred form of the invention, the hydrogen chloride or hydrochloric acid is either partially or entirely formed directly in the recycling catalyst solution of cupric and ferric ions by reaction of chlorine and hydrogen cyanide, either with or without pressure.
摘要:
Glycide is prepared by reacting allyl alcohol with hydrogen peroxide in the presence of a tungsten compound as a catalysts the excess allyl alcohol and the greatest part of the water distilled off, the sump mixture obtained in the distillation is split at 110.degree.-220.degree. C. and 5 to 60 torr in a thin layer evaporator into a volatile portion which is predominantly glycide, high boiling by products and the residual part of the water and a sump portion of glycerine, polyglycerine and catalysts. The volatile liquid portion is broken into glycide, water and high boiling byproducts at 5 to 60 torr in a distillation apparatus directly connected to the thin layer evaporator.