摘要:
The invention relates to a method for producing amino- or hydroxybenzonitriles during which, within the scope of an ammonolysis, the corresponding amino- or hydroxybenzoic acid compounds are reacted with ammonia in the presence of a phosphate-containing supported catalyst at temperatures between 250 °C and 500 °C. The actual production step is carried out in a reaction gas (mixture) and without the involvement of an organic solvent and is followed by an at least 2-stage purification step. Firstly, the gaseous mixture obtained from the production step is converted into an aqueous basic suspension, and the product contained in the solid matter is subsequently released from this suspension. The main advantage of this combined method is that it does not start by using esters which is why the obtained products, in contrast to conventional methods, are free of the otherwise usual by-products whereby leading to a high product purity. In addition, the claimed method can be carried out in the utmost economical manner since the final product and the by-products in the used suspension exist in different states of aggregation and, therefore, can be easily separated from one another. This makes it possible to obtain solvent-free benzonitriles, which contain amino or hydroxy groups, with a high yield and with a distinctly improved product quality.
摘要:
The invention relates to a method for isolating methyl glycine nitrile-N,N-diacetonitriles (MGDN) from an MGDN-containing aqueous emulsion with an MGDN content of 3 - 50% by weight in a crystallizer. The inventive method is characterized by (a) cooling the aqueous emulsion, starting from a temperature above the solidification point, to a temperature below the solidification point, the cooling rate in the temporal mean not exceeding 5 K/h, until substantially the total amount of the emulsified MGDN has solidified; and (b) continuing to cool the aqueous suspension obtained and/or concentrating it, the cooling rate being higher than that in step (a).
摘要:
Acrolein is removed from a process stream such as a process stream generated in the manufacture of acrylonitrile. The process includes reacting the acrolein with a compound containing a reactable thiol or hydroxyl moiety in the presence of an acid catalyst. The present process provides for a refined process stream that contains no more than 5 ppm by weight unreacted acrolein.
摘要:
The invention relates to a method of separating and isolating an acylated derivative of 4-[(S)-4-dimethylamino-1-(4-fluorophenyl)-1-hydroxybutyl]-3-hydroxymethylbenzonitrile by reaction of a mixture of the 4-[(S)-4-dimethylamino-1-(4-fluorophenyl)-1-hydroxy-butyl]-3-hydroxymethylbenzonitrile and an acylated derivative thereof with a compound which form a derivative of the 4-[(S)-4-dimethylamino-1-(4-fluorophenyl)-1-hydroxy-butyl]-3-hydroxymethylbenzonitrile containing a carboxylic acid group. The acylated derivative containing a carboxylic acid group precipitates once it is formed and may easily be separated from the reaction mixture.
摘要:
A method for producing a purified 2-cyanoacrylate is characterized in that distillation is conducted in the presence of a polymerization inhibitor whose boiling point is within ±12°C of the boiling point of the 2-cyanoacrylate. With this method, polymerization of 2-cyanoacrylate can be continuously prevented in the distillate system during distillation of a crude 2-cyanoacrylate, so that a purified 2-cyanoacrylate can be obtained.
摘要:
The present invention contemplates a process for the removal of impurities comprising amides, but which may include other impurities such as amines, from a solution of the nitrites and impurities. A reaction mixture is first formed and to that reaction mixture, 0.5 to 3wt% of approximately 60% H2SO4 is stirred in at room temperature and atmospheric pressure for a time effective for the removal of the amide impurities. Typically, after about 30 minutes, the amide impurity is removed into the lower, dark acid layer, probably as a salt. The remaining nitrile, after decantation or filtration, is still colored but is substantially free of amide. In a to second step, at room temperature or at a temperature of up to ~80°C, color can be removed from the nitrile by stirring the acid-washed nitrile with 0.5-5 wt% of clay (bentonite), charcoal, zeolitic type materials, mixtures thereof and the like.
摘要:
The invention relates to a method for reducing the content of an aliphatic, monounsaturated amine (IV) in a mixture (V) containing an aminonitrile (I) or a diamine (II) or a dinitrile (III) or mixtures thereof and amine (IV), whereby: a) mixture (V) is reacted with an anionic nucleophile (VI) in a quantity ranging from 0.01 to 10 mols per mol of amine (IV) in mixture (V) at a temperature ranging from 50 to 200 °C while obtaining mixture (VII), and; b) amino nitrile (I) or diamine (II) or dinitrile (III) or mixtures thereof are removed by distillation from mixture (VII) at a temperature ranging from 50 to 200 °C and under a pressure ranging from 0.1 to 100 kPa while obtaining a bottom product (VIII). The inventive method is characterized in that: c) an amino nitrile (I) or diamine (II) or dinitrile (III) or mixtures thereof are removed by distillation from bottom product (VIII) at a temperature which is lower than that selected in step b).
摘要:
The present invention relates to a continuous process for the cyanation of hydrogenated β-ketoesters in a cyanation zone maintained under conditions of temperature and pressure effective for cyanation of a hydrogenated R-ketoester. A substrate comprising a hydrogenated β-ketoester is continuously supplyed to the cyanation zone together with a cyanide. The substrate is contacted with the cyanide in the cyanation zone for a period effective for at least partial cyanation of the hydrogenated β-ketoester and a product stream is continuously extracted from the cyanation zone.
摘要:
Disclosed is a process for the preparation and recovery of cyclopropylacetonitrile by a novel combination of process steps beginning with a mixture of cyclopropylmethyl halide, a cyclobutyl halide and a 4-halo-1-butene. The process permits the recovery of substantially pure cyclopropylacetonitrile and cyclobutyl halide, e.g., cyclopropylacetonitrile and cyclobutyl halide each having a purity greater than 95 %.