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United States Patent (19) (11 3,954,955 Furkert (45) *May 4, 1976

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United States Patent (19) (11 3,954,955 Furkert (45) *May 4, 1976 United States Patent (19) (11 3,954,955 Furkert (45) *May 4, 1976 54 PROCESS FOR WORKING UP THE WASH Engineering, Duan Nostrand Co., N.Y., N.Y., 1932, SOLUTION OBTAINED IN THE WASHING pp. 1-3. OF SOCONTAINING OFF-GASES 75) Inventor: Herbert Furkert, Grosskonigsdorf, Primary Examiner-Oscar R. Vertiz Germany Assistant Examiner-Gary P. Straub 73) Assignee: Davy Powergas GmbH, Attorney, Agent, or Firm-Millen, Raptes & White Cologne-Braunsfeld, Germany * Notice: The portion of the term of this patent subsequent to Mar. 5, 1991, 57 ABSTRACT has been disclaimed. In a process which comprises scrubbing an SO 22 Filed: Aug. 30, 1972 containing gas with an aqueous ammonia solution to form ammonium sulfite and ammonium bisulfite as re (21) Appl. No.: 284,709 action products, neutralizing said reaction products Related U.S. Application Data with sulfuric acid to form SO, and aqueous ammo nium sulfate, and concentrating the resultant aqueous 63 Continuation-in-part of Ser. No. 228,258, Feb. 22, ammonium sulfate by evaporation, the improvement 1972, Pat. No. 3,795,731. which comprises: 30 Foreign Application Priority Data a heating the concentrated aqueous ammonium sulfate to a temperature of 900-1250°C in a Aug. 31, 197 Germany............................ 2143444 combustion chamber burning a carbon or sulfur containing fuel, in the presence of sufficient 52 U.S. Cl.............................. 423/541 A; 423/242 oxygen to maintain an oxygen content of 1-10 vol (5) Int. Cl..................... C01B 17160; C01B 17/50 % in the gas exiting from the combustion (58) Field of Search........... 423/522,539, 541, 542, chamber, to form a hot split gas consisting 4231544, 545, 547, 550, 242, 523 essentially of sulfur dioxide, sulfur trioxide, molecular nitrogen, molecular oxygen and water (56) References Cited vapor; and UNITED STATES PATENTS b. heat exchanging the hot split gas with the 1823,372 9, 1931 Merriam............................. 4231522 aqueous ammonium sulfate to evaporate the 2,406,930 9/1946 Titlestad ...... - ... 423/522 aqueous ammonium sulfate to a concentrate 2,862,789 12/1958 Burgess............ 423.1550 having a water content of less than 55 wt.%, 3.275,407 9/1966 Furkert et al.... ... 4231540 thereby cooling said hot split gas. 3,321,275 5/1967 Furkert et al.... ... 4231540 3,359,069 2/969 Furkert et al.... r 4231540 The split gas can be furhter worked up for any 3,383,70 5/1968 Furkert et al....................... 423154 purpose which an SO-containing gas is suitable, e.g., 3,645,683 2/1972 Isbell, Jr. ............................ 423/540 for the production of sulfuric acid. OTHER PUBLICATIONS Olsen J. C., Unit Process and Principles of Chemical 8 Claims, 1 Drawing Figure COOLNG EWAPORAT or Tower SCRU8BER PRECIPITATOR FuRNACE NH CONTACT PANT ACduation WESSE U.S. Patent May 4, 1976 3,954,955 9NITOOO 83MAOJ NOILýTnQ1ow (t HN) TESSEA 3,954,955 2 1 content of the feed. The price of ammonia decides whether combustion of ammonium salts of sulfur acids PROCESS FOR WORKING UP THE WASH into N, HO and SO, (U.S. Pat. No. 3,359,069) is more SOLUTION OBTANED IN THE WASHING OF economical than recovery of NH and SO, (U.S. Pat. SO,-CONTAINING OFF-GASES Nos. 3,321,275 and 3,383, 170). The present U.S. pa tent application describes a technical and economical CROSS REFERENCE TO RELATED APPLICATION improvement of the process (U.S. Pat. No. 3,359,069) This application is a continuation-in-part of copend applied for solutions containing ammonium salts of ing, commonly assigned U.S. patent application Ser. sulfur acids obtained in the SO,-containing off-gases. No. 228,258 filed Feb. 22, 1972, now U.S. Pat. No. 10 OBJECTS OF THE INVENTION 3,795,731. Accordingly, it is an object of this invention to pro BACKGROUND OF THE INVENTION vide an environmentally harmless process for the dis The present invention relates to a process for work posal of the wash solution obtained by washing SO,- ing up the wash solution obtained in the washing of 15 containing gas by adding ammonia. SO,-containing off-gases, which can also contain SO, Another object of this invention is to provide a pro using ammonia. cess for recovering the sulfur values of such wash solu It is known to wash SO-containing gases, e.g., the tions in a thermally efficient manner. end gas from a plant for the production of sulfuric acid A further object of this invention is to provide a by the contact process, or flue gas from the combustion 20 process for the production of SO-containing gas suit of sulfur containing fuels, by adding ammonia or an able for use in the contact process of preparing sulfuric aqueous ammonium hydroxide solution to the wash acid. solution. The ammonium hydroxide solution can con Other objects and advantages of this invention will tain generally 10-30 wt.% NHOH. The wash solution become apparent to those skilled in the art upon fur contains primarily ammonium sulfite and ammonium 25 ther study of the specification and appended claims. bisulfite. The washing process can be conducted in a SUMMARY OF THE INVENTION variety of ways, e.g. by contacting the SO-containing gas countercurrently with an aqueous ammonium sul Briefly, the above and other objects are attained in fites-containing spray, generally but not necessarily at a one aspect of this invention by providing, in a process temperature of 40° to 60°C and a pressure of about one 30 which comprises scrubbing an SO-containing gas with atmosphere. an aqueous ammonia solution to form ammonium sul In so far as the off-gas also contains sulfur trioxide, or fite and ammonium bisulfite as reaction products, neu an oxidation potential for oxidation of sulfite to sulfate tralizing said reaction products with sulfuric acid to exists, the wash solution can also contain ammonium form SO, and aqueous ammonium sulfate, and concen 35 sulfate. trating the resultant aqueous ammonium sulfate by U.S. Pat. No. 3,321,275 describes a process for the evaporation, the improvement which comprises: disposal of this wash solution in an environmentally a. heating the concentrated aqueous ammonium sul harmless manner. Hence it is known to acidify the fate to a temperature of 900-1250° C in a combustion solution by adding ammonium hydrogen sulfate, chamber burning a carbon or sulfur containing fuel, in whereby SO, is liberated, to evaporate the solution for 40 the presence of sufficient oxygen to maintain an oxygen recovery of the ammonium sulfate from the solution, content of 1-10 vol% in the gas exiting from the com and, in stages, to split it into ammonia and SO. This bustion chamber, to form a hot split gas consisting process indeed permits the recovery of the ammonia essentially of sulfur dioxide, sulfur trioxide, molecular required for the off-gas washing; but it requires a con nitrogen, molecular oxygen and water vapor, and siderable capital expenditure for the necessary multi- 5 b. heat exchanging the hot split gas with the aqueous stage plant. amonium sulfate to evaporate the aqueous ammonium U.S. Pat. No. 3,359,069 describes a process for the sulfate to a concentrate having a water content of less production of sulfur dioxide-containing gases by the than 55 wt.%, thereby cooling said hot split gas. thermal decomposition of waste sulfur acids and their The heat-exchanged split gas which serves as a car ammonium salts in the presence of oxygen. These 50 rier for the removal of water from the evaporation waste sulfur acids contain, for example, 34 wt.% water stage (b) can be further cooled by scrubbing with sulfu while solutions coming from washing off-gases contain ric acids of medium concentration formed from the about 55 wt.% water. The thermal decomposition of sulfur trioxide content in the split gas, which sulfuric such wash solutions results in split gases which are too acid can be used for the neutralization step. Additional poor in SO, for an economic production of sulfuric 55 split gas can be cooled to condense a large portion of acid. Combustion of sulfur or hydrogen sulfide in order the water vapor therefrom, and the condensate can be to increase the SO, content of the spent gas would disposed of as an effluent. result an unacceptable compulsory production of sulfu In one aspect, the present process has additional ric acid. advantages in that the neutralization and heat exchange U.S. Pat. No. 3,383, 170 describes a process for re 60 techniques can be simultaneously carried out in a single covering ammonia in yields of at least 95% from feeds combined stage. The neutralization by the addition of containing ammonium sulfate and/or ammonium bisul recycled sulfuric acid can be omitted if the split gas has fate by heating to temperatures of 200-450°C. NH is a sufficient sulfur trioxide content to form sulfuric acid produced from the decomposition of ammonium sul in the heat exchange step. fate, whereafter ammonium bisulfate is reduced to the BRIEF DESCRIPTION OF THE DRAWING bisulfite, which reacts to form SO, and ammonium sulfate; the process is controlled so that the amounts of The above and other objects of this invention will NH and SO, correspond to the initial NH and SO become more fully apparent to those skilled in the art 3,954,955 3 4 from the following detailed discussion, taken in con The hot split gas is preferably the SO-containing junction with the annexed Drawing, which schemati gaseous reaction product obtained by heating ammo cally illustrates the flow sheet of a plant suitable for nium sulfate at a temperature of 900-1250°C by com carrying out the process of this invention.
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