Method and device for removing contaminants arising during the production of aliphatic nitrate esters
AssigneeJosef Meissner GmbH & Co. KG
InventorsJürgen Pöhlmann, Heinrich Hermann, Mïrko Händel, Jürgen Gebauer
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Abstract
The invention relates to a method and to a device for removing contaminants arising during the production of aliphatic or alicyclic nitric acid esters, in particular for removing contaminants from nitrated crude nitric acid esters, which nitrated crude nitric acid esters arise during the nitration of monovalent or multivalent aliphatic or alicyclic alcohols capable of nitration, after the separation of the final nitrating acid, and to a production system for nitrating monovalent or multivalent aliphatic alcohols capable of nitration with subsequent purification of the nitrated nitric acid esters.
Claims20
A method for removing impurities including residual nitrating acid from a crude nitric ester obtained in the nitration of nitratable monohydric or polyhydric aliphatic or cycloaliphatic alcohols, the method comprising:
- removing the residual nitrating acid from the crude nitric ester, via treatment with at least one first washing medium;
- introducing the crude nitric ester and at least one second washing medium into and through at least one dispersing device for contacting and forming an emulsion of the crude nitric ester to be purified;
- introducing the emulsion into and through a device arranged downstream of the dispersing device, the device comprising a tube reactor, wherein the tube reactor is equipped with mixing elements for introducing additional mixing energy, so the impurities initially present in the crude nitric ester are at least partially removed during passage of the emulsion through the tube reactor and are at least partly transferred into the washing medium and neutralized thereby during passage of the emulsion through the tube reactor;
- and
- separating the nitric ester from the impurities downstream of the tube reactor, in a separation device for separating the nitrated products from the washing medium containing the impurities.
A method for the preparation of a nitric ester of a monohydric, a polyhydric aliphatic, or a cycloaliphatic alcohol via nitration of the monohydric, the polyhydric aliphatic, or the cycloaliphatic alcohol to form a crude nitrated product and subsequent purification of the crude nitrated product formed in the nitration, wherein the method comprises the steps of:
- (a) nitrating the monohydric, the polyhydric aliphatic, or the cycloaliphatic alcohol utilizing a nitrating acid in a nitration unit including one or more reaction vessels configured for carrying out a nitration reaction to form a crude nitrated product;
- (b) removing the residual nitrating acid from the crude nitrated product in a first separation device arranged downstream from the nitration unit and configured for the removal of the residual nitrating acid to form a crude nitric ester;
- (c) washing the crude nitric ester with a washing medium in a production line arranged downstream of the first separation device, the production line including a washing facility for carrying out the washing of the crude nitric ester including impurities,
- wherein the washing facility comprises:
- at least one dispersing device for contacting and emulsifying the crude nitric ester to be purified and a washing medium, to provide an emulsion comprising the crude nitric ester and the washing medium;
- and,
- a tube reactor for introducing the emulsion comprising the crude nitric ester to be purified and the washing medium and produced in the dispersing device, wherein the tube reactor is arranged downstream of the dispersing device and is equipped with mixing elements for introducing additional mixing energy, so that the impurities initially present in the crude nitric ester are at least partially removed during passage of the emulsion through the tube reactor and the impurities initially present in the crude nitric ester are at least partly transferred into the washing medium and neutralized thereby during passage of the emulsion through the tube reactor;
- and
- (d) separating the nitric ester from the washing medium containing the impurities, in a second separation device arranged in the production line downstream of the washing unit.
A method for the preparation of a nitric ester of a monohydric, a polyhydric aliphatic, or a cycloaliphatic alcohol via nitration of the monohydric, the polyhydric aliphatic, or the cycloaliphatic alcohol to form a crude nitrated product and subsequent purification of the crude nitrated product formed in the nitration, wherein the method comprises the steps of:
- (a) nitrating the monohydric, the polyhydric aliphatic, or the cycloaliphatic alcohol utilizing a nitrating acid in a nitration unit including one or more reaction vessels configured for carrying out a nitration reaction to form a crude nitrated product;
- (b) removing the residual nitrating acid from the crude nitrated product in a first separation device arranged downstream from the nitration unit and configured for the removal of the residual nitrating acid to form a crude nitric ester;
- (c) washing the crude nitric ester with a washing medium in a production line arranged downstream of the first separation device, the production line including a washing facility for carrying out the washing of the crude nitric ester including impurities,
- wherein the washing facility comprises:
- at least one dispersing device for contacting and emulsifying the crude nitric ester to be purified and a washing medium, to provide an emulsion comprising the crude nitric ester and the washing medium;
- and,
- a tube reactor for introducing the emulsion comprising the crude nitric ester to be purified and the washing medium and produced in the dispersing device, wherein the tube reactor is arranged downstream of the dispersing device and is equipped with mixing elements for introducing additional mixing energy, so that the impurities initially present in the crude nitric ester are at least partially removed during passage of the emulsion through the tube reactor and the impurities initially present in the crude nitric ester are at least partly transferred into the washing medium and neutralized thereby during passage of the emulsion through the tube reactor;
- (d) introducing the crude nitric ester, and the washing medium into a stirred vessel downstream of the washing facility to increase the contact and residence time between the crude nitric ester and the washing medium;
- and
- (e) separating the nitric ester from the washing medium containing the impurities, in a second separation device arranged in the production line downstream of the stirred vessel.
Dependencies are inferred from the claim text.