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United States Patent (19) 3,728,439 Urban |45 Apr

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United States Patent (19) 3,728,439 Urban |45 Apr United States Patent (19) 3,728,439 Urban |45 Apr. 17, 1973 54 TREATMENT OF A SULFTE Primary Examiner - Oscar R. Vertiz CONTAINING AOUEOUS STEAM TO Assistant Examiner-George O. Peters SELECTIVELY PRODUCE Attorney-James R. Hoatson, Jr. and Thomas K. Mc ELEMENTAL SULFUR Bride 75) Inventor: Peter Urban, Northbrook, Ill. 57 ABSTRACT (73) Assignee: Universal Oil Products Company, An input water stream containing a water-soluble Des Plaines, Ill. sulfite compound is treated to produce elemental sul 22 Filed: Nov. 5, 1970 fur, while minimizing the formation of undesired sulfate by-products by the steps of: (a) selectively con (21) Appl. No.: 87,393 verting the sulfite compound to the corresponding thiosulfate compound; (b) reacting a portion of the (52) U.S. C. .....................423.1567,210/50, 4231571 resulting thiosulfate-containing stream with a reducing (51) Int. Cl. .............................................C01b 17/02 agent to form a sulfide-containing stream; (c) reacting 58 Field of Search.................. 23/224, 229; 210/50, the remaining portion of the thiosulfate-containing 20/63 stream with the sulfide-containing stream to form the corresponding polysulfide compound; and thereafter, subjecting the resulting stream containing the polysul (56) References Cited fide compound to decomposition conditions selected UNITED STATES PATENTS to form elemental sulfur, hydrogen sulfide, and a sub 1,636,106 7/1927 Naef.......................................23/137 stantially sulfate-free treated water stream. The prin cipal utility of this treatment procedure is associated 3,536,618 Of 1970 Urban et al..... ...23/224 X with the clean up, or regeneration, of sulfite-contain 1,062,120 5/1913 Sanborn................................. 23/225 ing aqueous streams such as are produced by contact ing SO2 -containing flue gas with a suitable aqueous FOREIGN PATENTS OR APPLICATIONS absorbent stream. Key features of this process are the 947,640 selective conversion of the sulfite compound to the lf 1964 Great Britain.......................... 23/225 corresponding thiosulfate compound, the subsequent reduction of a portion of this thiosulfate compound to OTHER PUBLICATIONS the corresponding sulfide compound and the use of Mellor; 'Comprehensive Treatise on Inorganic and this sulfide compound to selectively reduce the Theoretical Chem...,' Longmans Green & Co., N.Y. remaining portion of the thiosulfate compound to ele 1930, Vol. X, pp. 516-518. mental sulfur. 20 Claims, 1 Drawing Figure 3,728,439 2 TREATMENT OF A SULFTE CONTAINING addition, the discharge of these gas streams into the at AQUEOUSSTEAM TO SELECTIVELY PRODUCE mosphere constitutes a waste of a valuable material ELEMENTAL SULFUR because the sulfur contained in same is an industrial commodity. The subject of the present invention is a multi-step Many processes have been proposed for removal of process for the selective treatment of an aqueous sulfur dioxide from these gas streams. A large percent stream containing a water-soluble sulfite compound for age of these proposed removal procedures involve con the purpose of converting the sulfite compound to ele tacting the sulfur dioxide-containing gas stream with an mental sulfur in a highly selective manner. Another aqueous absorbent stream which typically contain purpose for the treatment procedure is to lower the 10 materials which chemically or physically react with the total sulfur content (i.e., total amount of sulfur con sulfur dioxide in order to absorb same into the liquid tained in the aqueous stream in any form, calculated on solution. A common procedure involves the use of a an elemental basis) of the aqueous input stream to the solution of an alkaline reagent such as ammonium point where it can be safely discharged into a suitable 5 hydroxide, sodium hydroxide, sodium carbonate, am sewer without causing a major pollution problem, or al monium carbonate and the like alkaline reagents, to ternatively, reused in the process or industrial activity produce a rich absorbent stream containing the cor which originally produced it. More precisely, the responding sulfite compound. Likewise, similar aque present invention involves a novel four step process for ous solution containing salts of sulfurous acid are treating an aqueous stream containing a water-soluble produced in many areas of modern industry such as in sulfite compound in which the sulfite compound is first 20 the chemical, petrochemical, pharmaceutical steel, selectively reduced to the corresponding thiosulfate paper, food, fertilizer, petroleum and the like indus compound, a portion of this thiosulfate compound is tries. then selectively reduced to the corresponding sulfide Because these water streams contain sulfite com compound and the resulting sulfide compound is then 25 pounds, their discharge into a waste water sewer can used to selectively reduce the remaining portion of the cause substantial, well-known water pollution problems thiosulfate compound to form the corresponding including excessive biological oxygen demand, poison polysulfide compound. Elemental sulfur is then easily ing of marine and plant life and the like. Regardless of recovered from the polysulfide compound via a con the source of these aqueous, sulfite-containing streams, ventional decomposition technique. In a narrower 30 aspect, the current invention involves a procedure for it is clear that there is a substantial need for a simple the treatment of an aqueous input stream containing and effective method for treating them in order to ammonium sulfite and/or ammonium bisulfite to selec allow their reuse in the processes which produced them tively produce elemental sulfur and a treated aqueous or their safe discharge into a suitable sewer. In addi output stream which has greatly reduced total sulfur 35 tion, it is most advantageous to recover the sulfur con content relative to the input stream. In another limited tained in these streams in the form of elemental sulfur aspect, the present invention relates to the treatment of because of the substantial market therefore. In the case an aqueous input stream, which is produced by where the treated water stream is to be recycled to the scrubbing a gas stream containing SO, with an aqueous process which produced the input water stream, it is absorbent solution containing a suitable alkaline re 40 generally required that the treated water stream be sub agent, in order to regenerate the rich solution while stantially free of sulfate compound. The reason for this simultaneously converting the absorbed sulfite com requirement is that these compounds, once formed, are pound to elemental sulfur and minimizing the amount very intractable and in a closed system tend to build up of undesired, intractable sulfate by-products formed. in the recycle water stream until finely divided solids A major problem encountered in areas of industry 45 are formed. These solids then can precipitate in the today is associated with the production of waste gas form of a scale or sludge which can foul the internals of streams containing sulfur dioxide. The problem essen the equipment using this recycle stream. For instance, tially involves the disposal of these waste gas streams when the treated stream is recycled to a gas scrubbing without causing substantial air pollution. This problem process, these sulfate compounds can cause severe cor is an extremely complex one because of the wide 50 rosion and erosion difficulties in the scrubbing equip variety of industrial sources that emit these sulfur diox ment, plus they can foul the internals of the scrubbing ide-containing gas streams. One of the more common means. When a drag stream is withdrawn from the sources is associated with the combustion of sulfur process and discarded or treated by a method such as containing fuels in boilers, internal combustion en crystallization, evaporation or filtration, to remove gines, heating units, etc. to produce flue or stack gas 55 these sulfate compounds, valuable alkaline reagent is streams containing sulfur dioxide. Similarly, waste gas typically lost from the system. Moreover, the yield of streams of this type are generally produced by other in sulfur recovered during the water treatment operation dustrial processes such as the smelting of sulfur-bearing is detrimentally affected by these sulfate by-products. ores, the refining of sulfur-containing crude oils, the One solution that has been proposed to the problem synthesis of sulfuric acid, the sulfonation of hydrocar 60 of treating these sulfite-containing water streams is the bons, the production of coke, the production of sulfur use of a suitable reducing agent to react with the sulfite in a Claus process, the production of paper via a wood compounds contained therein to make elemental sulfur pulping process and the like industrial processes. It is and/or the corresponding sulfide compound. However, well known that the indiscriminate discharge of these despite stringent precautions, when common reducing gas streams into the atmosphere results in a substantial 65 agents such as hydrogen, a suitable sulfide compound, air pollution problem because the sulfur dioxide has ex or carbon monoxide are used in an attempt to directly tremely detrimental effects on animal and plant life. In reduce these sulfite compounds to elemental sulfur or 3,728,439 3 4. the corresponding sulfide compounds, undesired rather than attempt to directly reduce the sulfite com sulfate compounds are formed in unacceptable pound to elemental sulfur in a one step
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