Abstract:
A separation and purification method of 2-nitroethanol, including: (a) reacting paraformaldehyde with nitromethane in the presence of a base to obtain a mixture of 2-nitroethanol (I), 2-nitro-1,3-propanediol (II) and tris(hydroxymethyl) nitromethane (III); and (b) selecting an extraction solvent in which 2-nitroethanol (I), 2-nitro-1,3-propanediol (II) and tris(hydroxymethyl) nitromethane (III) are different in solubility; adding the extraction solvent to the mixture followed by extraction, separation, and vacuum concentration to obtain the 2-nitroethanol (I).
Abstract:
The present invention relates to a method for purifying raw dinitrotoluenes resulting from dinitration of toluene in the presence of a nitric acid/sulfuric acid/nitrating acid mixture, and a device or plant for performing the method, and a corresponding production plant for producing dinitrotoluene, characterized in that (a) the raw dinitrotoluenes are first subjected to a wash with at least one washing medium after separation of the nitrating acid mixture, followed by a separation of the washing medium; and that (b) subsequently the washed dinitrotoluenes resulting from method step (a) are subjected to stripping (stripping gas treatment) with at least one gas (stripping gas).
Abstract:
Process for scrubbing a crude mixture which is obtained in the nitration of toluene after separating off the nitrating acid and comprises dinitrotoluene, nitric acid, nitrogen oxides and sulfuric acid, which comprises two scrubbing steps (WS-I) and (WS-II), whereini) in a first scrubbing step (WS-I), the crude mixture is extracted with a scrubbing acid I comprising nitric acid, nitrogen oxides and sulfuric acid in a scrub comprising at least one extraction stage, where the scrubbing acid discharged from the first extraction stage (WS-I-1) of the first scrubbing step (WS-I) has a total acid content of from 10 to 40% by weight and a content of from 80 to 350 ppm of hydrocyanic acid, giving a prescrubbed crude mixture,ii) in a second scrubbing step (WS-II), the prescrubbed crude mixture comprising dinitrotoluene is extracted with a scrubbing acid II in a scrub comprising at least one, preferably at least 2, extraction stage(s), where the scrubbing acid discharged from the first extraction stage (WS-II-1) of the second scrubbing step (WS-II) has a pH of less than or equal to 4, giving a dinitrotoluene-comprising mixture which is essentially free of nitric acid, sulfuric acid, nitrogen oxides and hydrocyanic acid and has a content of not more than 300 ppm of nitric acid and nitrogen oxides, not more than 3 ppm of sulfate and not more than 50 ppm of hydrocyanic acid.
Abstract:
The present invention provides a process for purifying a monoterpene or sesquiterpene having a purity greater than about 98.5% (w/w). The process comprises the steps of derivatizing the monoterpene (or sesquiterpene) to produce a monoterpene (or sesquiterpene) derivative, separating the monoterpene (or sesquiterpene) derivative, and releasing the monoterpene (or sesquiterpene) from the derivative. Also encompassed by the scope of the present invention is a pharmaceutical composition comprising a monoterpene (or sesquiterpene) having a purity greater than about 98.5% (w/w). The purified monoterpene can be used to treat a disease such as cancer. The present monoterpene (or sesquiterpene) may be administered alone, or may be co-administered with radiation or other therapeutic agents, such as chemotherapeutic agents.
Abstract:
The present invention provides a process for purifying a monoterpene or sesquiterpene having a purity greater than about 98.5% (w/w). The process comprises the steps of derivatizing the monoterpene (or sesquiterpene) to produce a monoterpene (or sesquiterpene) derivative, separating the monoterpene (or sesquiterpene) derivative, and releasing the monoterpene (or sesquiterpene) from the derivative. Also encompassed by the scope of the present invention is a pharmaceutical composition comprising a monoterpene (or sesquiterpene) having a purity greater than about 98.5% (w/w). The purified monoterpene can be used to treat a disease such as cancer. The present monoterpene (or sesquiterpene) may be administered alone, or may be co-administered with radiation or other therapeutic agents, such as chemotherapeutic agents.
Abstract:
The present invention relates to a method for removing impurities from nitrated crude products obtained during the nitration of nitratable aromatic compounds, after removal of the final nitrating acid, by treatment with a washing medium, and also to a plant or apparatus suitable for implementing this method. Further provided by the invention is a production plant for the nitration of nitratable aromatic compounds with subsequent purification of the nitrated products.
Abstract:
A process for the continuous production of a compound of Formula (II), HO—R1—ONO2 (II) wherein R1 is a straight chain alkyl radical having from 3 to 6 carbon atoms, in a two-phase solvent system, comprising contacting a compound of Formula (I), HO—R1—OH (I) wherein R1 is as defined above, with nitric acid in the presence of a first solvent, wherein the compound of Formula (II) is continuously extracted into a second solvent, and the reaction is carried out in a mixing microreactor which provides a power loss of at least 1.3 times the power loss provided under identical conditions by a circular cross-section straight-channel microreactor having an internal diameter equal to the average hydraulic diameter of the mixing microreactor and a length equal to the length of the mixing microreactor.
Abstract:
A method of removing alkalinity and salt from a nitroaromatic product downstream of water washing to remove mineral acids and alkaline washing to remove salts of organic acids, comprises washing the product stream with an acidic aqueous solution, prior to the step of removing excess organic reactant, by steam stripping or distillation. Acid removed from the stripper or column is recycled back for use in the acidic washing. The acidic washing is done instead of the neutral washing step of the prior art. It removes residual salt and decreases the level of entrained colloidal water in the nitroaromatic product.
Abstract:
The invention relates to a method of preparing a high-purity nitrophenol and, more specifically, p-nitrophenol from a nitrohalobenzene. The inventive method comprises the following steps: (a) hydrolysis of a nitrohalobenzene compound by reacting said compound with a base; (b) acidification in order to produce the nitrophenol compound from the salt thereof by means of an acid treatment; (c) crystallisation of the nitrophenol compound obtained; and (d) separation of the product obtained. The invention is characterised in that it also comprises at least the following steps: (e) concentration of the reaction medium after hydrolysis (a) and before acidification (b); and (f) liquid/liquid decantation after acidification (b) and before crystallisation (c), which is intended to eliminate the water phase obtained after acidification (b).
Abstract:
Ammonium picrate, Explosive "D", is converted to picric acid, which is then converted to triaminophenol by the conversion of the aromatic nitro groups to amino groups. The triaminophenols are then converted to triaminobenzenes by the removal of the hydroxyl groups and the triaminobenzenes are converted to m-phenylenediamine, aniline, and primary aliphatic amines by the removal of amino groups.