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United States Patent (19) | 1 || 3,975,503 Hauschild Et Al

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United States Patent (19) | 1 || 3,975,503 Hauschild Et Al United States Patent (19) | 1 || 3,975,503 Hauschild et al. |45| Aug. 17, 1976 (54) METHOD FOR PRODUCING ALKAL 3.25.49.46 6/1966 Hass et al. .......................... 423f42 3644()89 2/ 1972 Minz et al........................... 423f4 CARBONATE 3,751.56() 8/1973 Neumann..... ... .42318.9 (75) Inventors: Ulrich Hauschild; Reimar Musall, 3,7739()2 11/1973 Neumann..... ... 42.3/421 both of Hannovcr; Hans-Jirgen 387 (),784 3/1975 Sueman............................... 4231431 Schröder, Pattensen, Hannover, all of Germany FOREIGN PATENTS OR APPLICATIONS 73,794 4/1968 Belgium.............................. 423/42 Assignee: Kali-Chemie Aktiengesellschaft, 229 3/1971 Japan..... ... 423f421 Hannover, Germany 2) 43 6/197l Japan..................... ... 4231421 89569() 5/1962 United Kingdom................. 423/42 Filcd: Dec. 13, 1974 Appl. No.: 532,365 Primary Examiner-Oscar R. Vertiz Assistant Examiner-Gary P. Straub Related U.S. Application Data Attorney, Agent, or Firn-Spencer & Kaye 63 Continuation of Ser. No. 436,719, Jan. 25, 1974, abandoned, which is a continuation of Ser. No. 204,058, Dec. 2, 1971, abandoned. 57) ABSTRACT A method for producing alkali carbonate crystals, in 3() Foreign Application Priority Data cluding adding to an alkali carbonate and alkali hy Dec. 8, 97 () Germany............................ 206()287 droxide solution stream a 10 to 75 weight-% alkali hy Aug. 27, 197 Germany............................ 243 ()()8 droxide solution, charging the resulting mixture into a CO-containing gas whose temperature is from 150 to 52) U.S. Cl.................................. 423/421; 423/189 700°C, collecting mixture remaining as liquid from the 51 int. Cl............................................ C01D 7/07 gas at the end of a residence time of mixture in gas of 58 Field of Search............................. 423/89, 421 0.1 to 10 seconds, separating alkali carbonate crystals from the collected mixture, and feeding the collected 56) References Cited mixture, following the separating, back in the alkali UNITED STATES PATENTS carbonate and alkali hydroxide solution stream for an 3, ()343 9/1963 Blumenthai......................... 423.1421 other adding of alkali hydroxide solution. 3.2()2,477 8, 1965 Leffler, Jr. et al................ 423142 3.22.848 ()/ 1965 Tasiaux............................... 423.1421 14 Claims, 1 Drawing Figure C02 NOH CONTAINING GAS SOLUTION 20 REACTION CHAMBER EXHAUST H20 CRYSTAL POOR STREAM COLLECTING CONTAINER SOLUTION OF NO2C03 -- No OH Na2CO3.H20, WET FLTRATE 2 DRYER COMBINING WESSEL Na2CO3 U.S. Patent Aug. 17, 1976 3,975,503 5 C02 NOOH CONTAINING GAS SOLUTION -b 3 4. 45 H20 2 3 REACTION CHAMBER 7 EXHAUST -- H20 4. CRYSTAL POOR STREAM COLLECTING CONTAINER . SOLUTION OF Na2CO3 Nabh CENTRFUGE 3 ity CRYSTAL-RICH STREAM Na2CO3.H20, WET FILTRATE S. DRYER 2 COMBINING G WESSEL Na2C03 3,975,503 1. 2 tion in Winnacker-Kiichler, CHEMISCHE TECH METHOD FOR PRODUCING ALKAL NOLOGIE, 3rd Edition (1970), Volume 1, page 222.) CARBONATE that the produced highly soluble potassium carbonate has been formed first dissolved in solution. The solu CROSS REFERENCE TO RELATED APPLICATION tion has had to be concentrated by evaporation. During This application is a continuation of copending appli cooling of the concentrated solution, hydrated potash cation Ser. No. 436,719, filed Jan. 25, 1974, which of formula KCO. 1% HO crystallizes. This is filtered itself is a continuation of application Ser. No. 204,058, and dried at 120°C to a commercial product containing filed Dec. 2, 1971, both now abandoned. 84 weight-% K2CO3. A product substantially free of 10 water of hydration and free of absorbed water is only BACKGROUND OF THE INVENTION obtained by drying at 250° to 350°C. The filtrate, con The present invention relates to a method for pro taining about 50 weight-% KCOa, is mixed with fresh ducing alkali carbonate from alkali hydroxide and car potassium lye and returned to the carbonating stage. bon dioxide. The previous practice for potassium carbonate pro The production of alkali carbonate from lye by reac 15 duction has not been satisfactory because, above all, tion with carbon dioxide or, more generally, carbon the solution concentrating and crystallizing of carbon dioxide-containing gases has won much interest in the ate require considerable expense for equipment. Be last two years. Due to the increasing need for chlorine cause of the strong temperature dependence of the in industry, increasing quantities of lye are becoming KCO-solubility, there have been difficulties for con available through the electrolysis of alkali choride solu 20 tinuous operation. Crystal precipitation often has led to tions. At least for a portion of this lye, there is no imme the plugging-up of pipe lines, valves, and other equip diate demand. met, The known methods for carbonating lyes have seri ous drawbacks. SUMMARY OF THE INVENTION A direct carbonating of the usual 50 weight-% so 25 An object of the invention, therefore, is to provide a dium hydroxide lye leads, for example, to encrustations method for the carbonating of both sodium and potas and crystal deposits at undesired spots in the apparatus sium lyes which, as compared with the methods previ during the conversion using carbon dioxide, and espe ously contemplated, is technically simple and which cially during the needed concentrating of the resulting operates economically. soda solution, by evaporation, after removal of the 30 This as well as other objects which will become ap precipitate. Moreover, the crystals of alkali carbonate parent in the discussion that follows are achieved, ac often trap within themselves impurities in the form of cording to the present invention, by a method for pro sodium hydroxide or the small metal particles which ducing alkali carbonate crystals, including adding to an are the result of wear. Even the process disclosed in alkali carbonate and alkali hydroxide solution stream a German Published Application (Auslegeschrift) No. 35 10 to 75 weight-% alkali hydroxide solution, charging 1,138,748, which operates in two stages, cannot elimi the resulting mixture into a CO2-containing gas whose nate these disadvantages. temperature is from 150 to 700°C, collecting mixture Evaporation of the excess water entering a process remaining as liquid from the gas at the end of a resi via the sodium lye may be carried out right in the car dence time of mixture in gas of 0.1 to 10 seconds, bonating stage, so that a special evaporating for con 40 separating alkali carbonate crystals from the collected centrating of the above-mentioned soda solution can be mixture, and feeding the collected mixture, following eliminated. Since the released heat of neutralization is the separating, back in the alkali carbonate and alkali not large enough to supply the heat needed to evapo hydroxide solution stream for another adding of alkali rate the requisite amount of water, the necessary en hydroxide solution. ergy must be supplied either before the reaction, for 45 example by strong heating of the high-percentage so BRIEF DESCRIPTION OF THE DRAWING dium lye according to German Laid-Open Application The sole FIGURE is a preferred flow diagram of the (Offenlegungsschrift) No. 1,567,921, or within the method according to the present invention. reactor such as in German Laid-Open Application (Of fenlegungsschrift). No. 1,811, 168 using steam coils. 50 DESCRIPTION OF THE PREFERRED The solids are continuously removed from the hot sus EMBODIMENTS pension, while the filtrate, which mainly contains soda, The present inventors have discovered a method for is fed back to the reactor. The carbon dioxide or car producing sodium carbonate, preferably in its monohy bon dioxide-containing gas is bubbled from below drate form, by reacting sodium lye with carbon dioxide through the reactor, which may for example be a car 55 or, more generally, carbon-dioxide-containing gases. bonating tower or container equipped with a stirring This method substantially avoids the difficulties of the device. previously contemplated methods as above-described. The above-described processes have the disadvan The method of the invention is characterized by the tages that they work with a relatively large liquid vol feeding of a 10 to 75 weight-% (i.e. grams NaOH per ume and require a not insignificant expense for electri 60 100 grams solution) aqueous sodium hydroxide solu cal energy. Additionally, should there be a failure tion to a continuously circulated aqueous solution of somewhere in the system to cause the liquid to become sodium carbonate and sodium hydroxide, by the charg still, then a critical situation immediately develops be ing of the resulting mixture into hot (150 to 700°C) cause crystals begin to settle in the carbonating con CO2, or CO-containing gas, as finely divided droplets tainer, pipe lines, pumps, etc., to cause a difficultly 65 of the resulting mixture, by collecting that portion of removable plugging-up of the system. the resulting mixture still remaining as liquid from the In the case of producing potassium carbonate, the gas after a residence time of the resulting mixture in the practice has been such (See, for example, the descrip gas of 0.1 to 10 seconds, by separating the formed, 3,975,503 3 4 easily filterable carbonate crystals from the collected burning processes, there is an excess of CO2 available, mixture, and by returning the collected mixture as the so that theoretically the entire NaOH charged to the continuously circulating aqueous solution of sodium reaction chamber could be transformed into sodium carbonate and sodium hydroxide. carbonate. According to the present invention, it is not According to a preferred embodiment of the method necessary and even not desired that the entire sodium of the invention, the collected liquid-phase mixture is lye charged to the reaction chamber be carbonated; the split into two streams and the formed crystals of sodium portion of the charged lye that is carbonated should be carbonate are removed by filtration from only one of equal to that combined with the sodium carbonate and the streams with the filtrate and the other stream then sodium hydroxide solution in the step of adding.
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