DE874000C - Process for processing ammonia water containing hydrogen sulfide - Google Patents

Description

Process for processing ammonia water containing hydrogen sulphide It has already been suggested to take ammonium sulfide by treating it with air Pressure and at elevated temperature to convert into ammonium sulfate. Although the transformation this practically runs quantitatively, the procedure has been extraordinary because of the slow reaction in technology cannot prevail. For this reason it was So far it has not been possible to use hydrogen sulphide or ammonium; sulphides Ammonia water, as is known in the case of dry distillation, is bituminous Fuels and similar processes incurred must be subjected to the same procedure. Nevertheless, such a process would have great economic importance, since it Path shows the inferior and ammonia polluting sulfides to salable To refine ammonium sulfate, quite apart from the fact that in this way the S O4- Ion of the ammonium sulfate is generated from the production's own sulfur.

It has now been found that the oxidation of ammonium sulfides to ammonium susfate in the shortest possible time and, moreover, in continuous operation can, if you take the sulfur, hydrogen-containing ammonia base at elevated temperature can trickle over a Füllkörper.schicht, which is located in a vessel, in which the oxidizing agent (air, oxygen or other oxygen-containing gases) is introduced under pressure. It is useful to use an in more suitable Way heated pressure column o &. Like. In which above the ammonia water to be treated is abandoned, while Tnan below the ammonia water now containing ammonium sulfate continuously withdraws.

If further found, one can see the reaction rate even increase if you take small amounts of heavy metal salts, such as the liquid Copper, nickel or cobalt chloride added. You can also use it as a filler It is advantageous to use coal-like substances such as charcoal, aldiv charcoal, coke, etc. the The level of pressure and temperature depends on the duration of contact with the oxidizing agent with the liquid and the hydrogen sulfide concentration of the ammonia water a'b, namely with longer contact time and lower hydrogen sulfide concentration Pressures from 5 to 10 atmospheres and temperatures around 100 degrees are sufficient, while -man for shorter ones Contact times and high hydrogen sulfide concentrations pressures up to 5o atü and temperatures Ibis needed to 170 °.

It should also be mentioned that there are also other oxidizable substances that may be present Sulfur compounds, such as polysulfide or thiosulfate, according to the one described Process can be oxidized to sulphate smoothly and in a short time.

Since in technical ammonia water the ammonia, for hydrogen sulphide, is generally present in a larger amount than is necessary for the formation of ammonium sulphate, the ammonium sulphate solution flowing out of the oxidation vessel usually contains a lot of free ammonia, which is expediently distilled off as pure ammonia adar compressed ammonia water wins. After the abortion. of the ammonia remaining ammonium sulphate solution is processed into solid salt in a known manner. Introductory examples i. In a vertical autoclave, 1 cbm of ammonia water per square meter with 21 kg N 11.3, 3.1 kg H 2 S and 18.5 kg C 02 in cocurrent with air at 25 atmospheres at 115 ° over a 3 m height; Packing layer consisting of rings passed. The liquid drawn out at the foot of the autoclave contained 12 kg of ammonium sulphate, 17.9 'kg' of free ammonia and 12.5 kg per cubic meter. Carbon dioxide, but no more substances that discolour iodine. . z. When using compressed ammonia water, which contained 13q.9 free ammonia, 24.8 g visual hydrogen and 10% carbon dioxide per liter, the complete oxidation to the sulfate at 50 atmospheric air and 165 ° was reached, whereby the solid column again 3 m high and 0.8 cbm of ammonia water per square meter and hour was passed in continuous operation. The ammonia water withdrawn at the foot of the autoclave contained 94 g ammonium sulphate, 1,039 free ammonia and 88 g carbon dioxide per liter. Iodine decolorizing substances could no longer be detected.

3. If the experiment of, Example 2 is repeated with the addition of. 0.2 g of carbon chloride per liter of ammonia water, see above. one achieves the iooo / o turnover to ammonium sulfate under otherwise identical conditions already at 25 atmospheres and 155 degrees.

4. If you use a filling instead of the filling made of rings those of activated charcoal, the hydrogen sulfide of an ammonia water with 139 g N H3, 34 g H2 S and 76 g C 02 per liter with a throughput of. o.8 cbm per Square meter and hour with 25 atm. Air at 150 ° quantitatively to sulfuric acid oxidized. A water is obtained which contains 132 g of ammonium sulfate and 99.5 g of free per liter. Animo: niak and 63 g of carbon dioxide.

Claims (3)

PATENT CLAIMS: i. Process for processing hydrogen sulphide containing ammonia water to obtain: ammonium sulphate and pure ammonia, characterized in that the starting liquid is at increased pressure and elevated temperature in the presence of, air, oxygen or other oxygen-containing Lets gases trickle over large-surface packing, from or now ammonium isu.lfat containing solution drives off the free ammonia and the remaining lye solid salt processed. 2. The method according to claim i, characterized in that that small amounts of heavy metal salts are added to the crude ammonia water before pressure oxidation clogs. 3. The method according to claim i and / dder 2, characterized in that one as fillers, coarse-grained, carbon-like substances such as activated carbon, charcoal, coke and the like, are used.