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United States Patent 9) 11, 3,935,100 Alagy Et Al

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United States Patent 9) 11, 3,935,100 Alagy Et Al United States Patent 9) 11, 3,935,100 Alagy et al. (45) Jan. 27, 1976 54) PROCESS FOR THE TREATMENT OF l,557, 88 10/1925 Newlands.............................. 20153 WASTE WATERS CONTAINING SULFURIC 1959,305 5/1934 Rentschler.......................... 423 fliS8 2,094,902 10/937 Muller ................................ 4231554 ACID AND/OR AMMONUM SULFATE 2,863,732 12/1958 Bowers et al..................... 20/50 X (75) Inventors: Jacques Alagy, Lyon; Christian 3,784,680 l/1974 Strong et al.................... 4231554 X Busson, Rueil Malmaison; Maurice Cessou, Communarg, all of France (73) Assignee: Institut Francais du Petrole, Paris, Primary Examiner-Thomas G. Wyse France Attorney, Agent, or Firm-Millen, Raptes & White (22) Filed: June 28, 1974 21 ) Appl. No.: 484,228 (57) ABSTRACT (30) Foreign Application Priority Data Process for treating a waste water containing sulfuric June 29, 1973 France.............................. 73.2427 acid and/or ammonium sulfate comprising (1) react Dec. 4, 1973 France .............................. 73.433 18 ing said water with barium sulfide to form barium sul Mar. 6, 1974 France .............................. 7408095 fate, (2) reacting the latter with carbon containing in organic impurities, at high temperature, thereby form 52 U.S. C. ...................... 210,45; 210/47; 210/48; ing barium sulfide, at least a major portion of which is 210/50; 423/158 recycled to step (1), and a gas which is separated, (3) (51 Int. Cl.’........................ C02B 1134; CO2C5/06 dissolving in water a minor portion of the barium sul 58) Field of Search.................... 210/42, 45, 47-53, fide produced in step (2), separating the insoluble im 210/63, 67, 71; 423, 158, 166, 170,554 purities therefrom and recycling at least one portion of the resulting purified solution to step ( ). (56) References Cited UNITED STATES PATENTS 24 Claims, 4 Drawing Figures 62404 5, 1899 Jacobs ................................ 423 ft 70 U.S. Patent Jan. 27, 1976 Sheet 1 of 4 3,935,100 22 FG.1 U.S. Patent Jan. 27, 1976 Sheet 2 of 4 3,935,100 F.G.2 51 5 l 1 2 12 34 33 3 O 42 S 3 P. t. 39 15 44 4. O-20 26 47 24 U.S. Patent Jan. 27, 1976 Sheet 3 of 4 3,935,100 FG.3 22 23 46 45 31 25 (2) 30 21 40 28 5 17. 32 1 2 12 42 "... 39 11 U.S. Patent Jan. 27, 1976 Sheet 4 of 4 3,935,100 3,935,100 1 2 from the insoluble impurities contained therein and (5) PROCESS FOR THE TREATMENT OF WASTE transferring at least one portion of the resulting puri WATERS CONTAINING SULFURIC ACID AND/OR fied solution to step (1). AMMONUM SULFATE BRIEF DESCRIPTION OF THE DRAWINGS In the course of numerous chemical operations and The invention is illustrated by the accompanying various treatments, solutions of sulfuric acid are used. drawings: The waste waters from said operations are polluted by FIG. 1 is a schematic flow diagram illustrating a first organic and inorganic impurities and by free sulfuric embodiment which may be used when treating rela acid whose concentrations are variable to a large ex O tively dilute sulfuric acid containing waste water; tent. FIG. 2 is a modification of the diagram of FIG. 1 The discharge of these waste waters resulting in a concerning the treatment of two different streams of pollution of waters, difficult problems have to be solved sulfuric acid containing waste water. by the industry in order to comply with more and more FIG. 3 is a modification of the diagram of FIG. 1 severe regulations in this field. As a matter of fact, this 15 concerning the treatment of relatively concentrated water cannot be sent to the plants usually used for the sulfuric acid containing waste water. treatment of waste waters, due to the presence of sulfu FIG. 4 is a modification of the diagram of FIG. 3 ric acid. The neutralization by CaO, as carried out in concerning the treatment of ammonium sulfate con numerous plants, requires to solve the problem of the taining waste water. discharge of the formed CaSO4. Other waste waters 20 contain ammonium sulfate. DETALED DESCRIPTION OF THE DRAWINGS According to a first embodiment, waste water is re SUMMARY acted in a first step with barium sulfide (BaS). The The object of this invention is to provide a general latter may be used, for example, as a powder or in method for treating such waste waters irrespective of 25 solution or suspension in water or in a gas. We prefera their origin and their concentration. This method per bly proceed with a slight shortage of barium sulfide mits to recover and recycle sulfur. It is particularly with respect to SO ions so that the pH during the oper convenient for treating waste waters of low sulfuric ation and particularly at the outlet of the neutralization acid content, for example from 1 to 40 percent by reactor is maintained between 3 and 7 and, preferably, weight. These waters may also contain soluble sulfates, 30 between 4 and 6. The reaction is preferably conducted for example ammonium sulfates or various metal sul in a stirred reactor in order to completely exhaust the fates. introduced BaS and to maintain in suspension the The optimum concentration being from 10 to 30 formed barium sulfate BaSO. The substantially pure percent b.w. , when various waste waters of different hydrogen sulfide (HS) produced by the reaction may origin are available, it is possible by admixing them, to be converted in a burner to sulfur dioxide (SO) which adjust the sulfuric content of the resulting mixture. can be used for example for manufacturing sulfuric When the total concentration is greater than 30 per acid. The HS may also be converted to sulfur, for cent by weight, we can proceed to a dilution by recy example by the Claus process. The precipitation of cling a portion of the treated water. However, in a BaSO may be conducted under atmospheric pressure particular embodiment, the treated waters contain 20 40 or super atmospheric pressure and at Toom tempera to 40 percent by weight of sulfuric acid or ammonium ture or a higher temperature. The residence time is sulfate. usually from 0.1 to 1 hour. A very significant parame The present process makes use of the known reaction ter of this reaction is the pH at the outlet of the reactor of reduction of barium sulfate to barium sulfide by which must be maintained below 7 in order to limit as means of carbon. It has however been observed that 45 much as possible the amount of soluble Ba, irrespective this process was difficult to carry out. For example, the of its form, in the medium and, preferably, to a value insoluble impurities accompanying the treated waters lower than 10 ppm by weight corresponding to the or resulting from the reacted materials, have the effect solubility of BaSO in water. of progressively reducing the efficiency of the process. In a second step, the resulting barium sulfate suspen Moreover, it has been observed that the gaseous efflu 50 sion in water is fractionated, for example filtrated with ents obtained at various points of the installation could or without filtration aids or dried or centrifuged. The not be discharged as such in the atmosphere, in view of solid precipitate consisting mainly of BaSO4, but also their polluting action. possibly, of other organic and inorganic impurities, is The present process provides an economical way of advantageously washed with water. solving these difficulties. 55 In a third step, this precipitate is intimately admixed The invention concerns a process for treating a waste with carbon possibly containing in organic impurities, water containing sulfuric acid and/or ammonium sul for example coal or coke or, preferably finely crushed fate, comprising the steps of : (1) reacting the waste petroleum coke. This mixture is treated in an oven water with barium sulfide, introduced at least partly in where BaSO is reduced at high temperature by the the solid state, so as to form a suspension of solid bar 60 carbon to BaS according to a well known process. We ium sulfate in waste water, (2) reacting the resulting proceed for example at a temperature of from 700 to barium sulfate at high temperature with carbon con 1 500°C. During this operation, the organic impurities, taining inorganic impurities so as to form solid barium if any, are incinerated and the inorganic impurities, as sulfide containing inorganic impurities) and a gas well as the coal ashes, are removed from the system by which is separated, (3) recycling to step (1) at least the 65 purging a portion of the produced BaS. At least the major portion of the formed solid barium sulfide and major portion (more than 50 percent) of the produced (4) dissolving in water a minor portion of solid barium BaS is recycled to the neutralization reactor. The sulfide from step (2), separating the resulting solution purged BaS fraction is defined by the amount of inor 3,935,100 3 4 ganic impurities, particularly ashes, to be removed about 16.9 T/h. The neutralization of HSO, by BaS is from the system and by the stationary concentration conducted under controlled pH, the latter being main compatible with a good operation of the oven. This tained at a value of at most 6. The average residence fraction is, for example from 5 to 30 percent by weight. time in the reactor is 0.25 h. in these conditions, the in a fourth step the purged BaS is treated with water, BaS attack is substantially complete. Through line 21, preferably at a temperature of 70-80°C, in order to 3.2 T?h of HS evolve which are subsequently con dissolve substantially all the BaS.
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