Krupp Koppers Gmbh

Martin Schulze

Gerhard Preusser

Gerd Emmrich

Klaus Richter

Hans-Christoph Schneider

Bernhard Firnhaber

Fritz Schwall

Wilhelm Huwels

In the method for the production of an aromate concentrate suitable for use as blending component for gasifier fuel, feed hydrocarbon mixtures having boiling ranges substantially between 40.degree. and 170.degree. C., are subjected, without any previous separation into individual fractions, to an extractive distillation employing N-substituted morpholine, substituents of which display no more than seven C-atoms, as selective solvent. Herewith, the lower boiling non-aromates with a boiling range up to about 105.degree. C., practically completely, and most of the higher boiling non-aromates with a boiling range between about 105.degree. and 160.degree. C., are recovered as raffinate, whereas the aromates, which are to be employed in whole or in part as blending component, come down in the extract of the extractive distillation. In order to separate heavy aromates from solvent, a partial stream of the circulating solvent is mixed with water, and the heavy aromates are separated as a light phase from the solvent-water mixture. The solvent-water mixture is then separated into its components, which are re-utilized.

Method for the production of an aromate concentrate suitable for use as

The process for production of an aromate concentrate for use as a blending component for gasification fuel includes subjecting another feed hydrocarbon mixture to an extractive distillation using N-substituted morpholines as selective solvent in a extractive distillation column. Low-boiling non-aromates with a boiling range up to about 105.degree. C. practically completely and higher-boiling non-aromates with a boiling range between about 105.degree. and 160.degree. C. to a substantial extent are discharged as a raffinate from the top of the extractive distillation column. The extract bottoms from the extractive distillation are fed to a solvent stripping column where the solvent is at least partially recovered from other hydrocarbons. To eliminate condensation and polymerization products due to components with a boiling point over 170.degree. C. from the feed hydrocarbon mixture which can impair the process, a feed hydrocarbon mixture which contains those high boiling components is predistilled prior to extractive distillation to remove them. The top product from the predistillation column is fed to the extractive distillation column for extractive distillation. The predistillation residue can then be added to other hydrocarbons to form the aromate concentrate.

Process for the production of an aromate concentrate suitable for use as

A method is disclosed for the separation of aromates from hydrocarbon mixtures employed as entry products, by means of extractive distillation, employing as selective solvent N-substituted morpholine, the substitutions of which display no more than 7 C atoms. The raffinate produced as top product of the extractive distillation is subjected to a distillation, whereby the produced sump product with a solvent content between 20-75% by weight and a temperature between 20.degree.-70.degree. C., is led into a separation container and there separated into a heavy and a light phase. The heavy phase is then recycled into the extractive distillation column, whereas the light phase is recycled into the raffinate distillation column.

Method for the separation of aromates from hydrocarbon mixtures

Disclosed is a method for recovering pure aromatic substances from a mixture of hydrocarbons containing both aromatic and non-aromatic fractions. The input mixture is fed through an extractive stage provided with a preliminary distillation column. In the preliminary stage the aromatics-containing product is treated at a pressure up to 20 bar and a temperature up to 300.degree. C. The pressure is adjusted to a value at which the operational temperature of the preliminary stage is higher than the pressure and temperature in the extractive stage and the heat of the vapors discharged from the preliminary stage is used for heating the extractive stage.

Method of recovering pure aromatic substances

A process and apparatus are provided controlling the heat input of an extractive distillation column. The bottom of the column is heated with a major stream of thermal energy which is either slowly varying in time or controlled by the amount of starting material mixture and with a minor stream of thermal energy which is controlled by sensing the thermodynamic state in the upper half of the column during the process. The major stream can provide about 90 percent and the minor stream about 10 percent of the heat fed to the column. The minor stream can be controlled by the temperature at one point in the upper half of the column, by the temperature difference at two points in the upper half of the column or by gas chromatographic analysis of the extract material concentration near the top of the column. The process allows one to keep a low concentration of the extract material in the raffinate.

Heat input control of an extractive distillation column

A method for working up residues of an extractive distilling process for obtaining pure hydrocarbons. The residue from an extractive distilling column is fed to the about middle part of a distilling column. The hydrocarbons are distilled and removed at the head of the distilling column and the solvent is removed at the bottom of the distilling column. A sidestream is removed from the distilling column at a position above the feed plate for the residue from the extractive distilling column via a so-called reflux evaporator plate having an elevated level of liquid. The sidestream is heated by indirect heat exchange with the solvent flowing from the distilling column. The heated-up sidestream is fed back into the distilling column at a level at or above the reflux evaporator plate. The concentration of the solvent at the reflux evaporator plate is controlled by the amount of reflux at the head of the distilling column. The heating of the side stream reduces the heat requirement of the bottom boiler of the distilling column by about 35 percent.

Extractive distilling with reworking of residue

In order to prevent corrosion of the apparatus in extraction and extractive distillation processes where N-substituted morpholine is employed as the selective solvent an additive is added to the solvent which additive consists of (a) phosphoric acid, (b) a salt thereof, (c) a vanadium compound, (d) a molybdenum compound or (e) a mixture of two or more of these compounds, the addition being effected in an amount of about 0.005 to 0.02% by weight of the morpholine solvent.

Process for operating extraction or extractive distillation _apparatus

Process for recovering highly pure aromatic substances from mixtures of hydrocarbons which contain in addition to the aromatic substances, large amounts of non-aromatic substances by liquid-liquid extraction in combination with an after arranged extractive distillation whereby the liquid-liquid extraction of the starting hydrocarbon mixture is carried out under such conditions that the resulting extract contains substantially the total amount of the aromatic substances and a portion of the non-aromatic substances, introducing this extract into an after arranged extractive distillation for further separating said extract whereby the sump product (extract phase) formed is drawn off and introduced into an after arranged distillation column where it is separated into an aromatic and a solvent fraction, while the head product of the extractive distillation (raffinate phase) is reintroduced into the bottom of the extractor for liquid-liquid extraction thereof, wherein there is used in both of the extracting stages, as selective solvent, morpholine and/or N-substituted morpholine in admixture with water whereby the water content of the solvent for the liquid-liquid extraction amounts to between 2-15 weight percent and for the extractive distillation amounts to between 0 and 8 weight percent.

Process for recovering highly pure aromatics from a mixture of aromatics

A hydrocarbon mixture consisting of an aromatic and a non-aromatic component is subjected to a liquid-liquid extraction and/or an extractive distillation. A solvent is used which selectively dissolves the aromatic component so as to form an extract phase. The extract phase is introduced into a distillation column for separating the solvent and the aromatic component. The column is provided with trays and the extract phase is introduced into the column at about the middle thereof from where the solvent flows downwardly and the aromatic component flows upwardly. Sufficient water is introduced into the sump of the column to insure that the trays above the location at which the extract phase enters the column are filled with water during the separation. This improves the operation of the distillation column. An arrangement for carrying out the above process is also disclosed.

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Neviges, Germany

Martin Schulze