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United States Patent (19) [11] 3,929,964 Thoma (45) Dec

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United States Patent (19) [11] 3,929,964 Thoma (45) Dec United States Patent (19) [11] 3,929,964 Thoma (45) Dec. 30, 1975 54) PROCESS FOR THE CONVERSION OF 3,846,535 l l 1974 Fonseca.............................. 4231422 SODIUM SULFTE 76 Inventor: Matthias Thoma, Primary Examiner-Oscar R. Vertiz Johann-Strauss-Strasse 8, 8264 Assistant Examiner-Gary P. Straub Waldkraiburg, Germany 22 Filed: Sept. 23, 1974 57 ABSTRACT 21 Appl. No.: 508,401 The sodium sulfite obtained as a byproduct in the pro duction of hydroxy aromatic compounds from aro 30 Foreign Application Priority Data matic hydrocarbons, sulfur trioxide and sodium hy Oct. 5, 1973 Germany............................ 2350.191 droxide, is converted into sulfur trioxide and sodium hydroxide for recirculation of same in said production 52 U.S. Cl. ................ 423/183; 4231166; 423/242; of hydroxy aromatic compounds, by a process 423/428; 423/438; 438/532; 4231555; wherein: (a) the sodium sulfite is reacted with zinc 423/642; 260/628 chloride to form sodium chloride and zinc sulfite; (b) 51 Int. Cl."............................................ C01D 1120 the zinc sulfite is heated to form zinc oxide and sulfur 58 dioxide and the sulfur dioxide is oxidized to sulfur tri 4231190, 422, 423, 424, 426, 427, 491, 499, oxide; (c) the sodium chloride is reacted with ammo 512,539, 541 A, 532,533, 622, 642, 643; nium bicarbonate to form ammonium chloride and so 260/628 dium bicarbonate; (d) the zinc oxide is reacted with the ammonium chloride to form zinc chloride and am 56 References Cited monia; (e) the ammonia is reacted in the Solvay Pro UNITED STATES PATENTS cess to form ammonium bicarbonate; and (f) the so 2,180,755 1 1/1939 Carrels et al...................... 423/643 dium bicarbonate is heated to form sodium carbonate 2,259,409 10/1941 Wenzel et al..................... 4231622 and carbon dioxide, and the sodium carbonate is re 2,927,001 3/960 McCulloush........................ 4231532 acted with calcium oxide to form sodium hydroxide. 3,329,479 7/1967 Hustinx......... ... 423190. 3,535,083 10/1970 Smith.................................. 423/242 6 Claims, No Drawings 3,929,964 2 Thus the progress of the present invention represents PROCESS FOR THE CONVERSION OF SODIUM a technical and economical progress also in this re SULFITE spect. The sodium carbonate obtained during the conver This invention relates to a process for converting sion step represents no problem concerning the pollu sodium sulfite into sulfur trioxide and sodium hydrox tion laws. Sodium carbonates are harmless and further ide. more sodium carbonates are required by numerous It is well-known that during the production of hy branches of industry. droxy aromatics from aromatic sulphonic acids with During the conversion of sodium sulfite by means of Sodium hydroxide equivalent quantities of sodium sul 10 zinc chloride on one hand sodium chloride is obtained fite are obtained as a by-product. which can be converted into soda by the generally On the basis of the present pollution regulations, known Solvay process or possibly, when using calcium hydroxide, also into sodium hydroxide. On the other sodium sulfite may be used in the production of cellu : hand the zinc sulfite formed in the conversion of so losic material only in a very small extent. For this rea 15 dium sulfite by means of zinc chloride is decomposed Son Sodium sulfite has to be utilized or removed in a on heating into sulphur dioxide and zinc oxide which is form corresponding to the pollution laws. reacted together with the ammonium chloride obtained A well-known method for processing sodium sulfite is in the Solvay process and which is used for the recovery its oxidation into sodium sulfate or its neutralization, by of zinc chloride. The reaction is practically quantita means of suitable acids, into sodium salts that can be 20 tive. The resulting ammonia, in turn, is used in the re-used. These procedures, however, are costly and Solvay process. Sulphur dioxide is oxidized into sulphur time-consuming and furthermore additional chemicals trioxide and is employed as such or as sulphuric acid are consumed. Moreover it has to be mentioned that up for the sulfonation step. to now no possibility has been found for the removal of This means: in this process the formation of unde Sodium sulfate simultaneously solving the pollution 25 sired by-products is completely prevented as the mate problem satisfactorily. rials required for the processing of sodium sulfite are The present invention is based on the task of supply recovered completely, i.e. practically quantitatively ing a non-pollution processing of sodium sulfite which during the process and the by-products obtained in the can be carried out simply without obtaining any by-pro conversion are consumed again completely, too... ducts. • 30 As already mentioned in the conversion of sodium According to this invention this aim is reached by sulfite according to the present invention exactly those converting sodium sulfite into sodium hydroxide and materials are recovered which are required in the man sulphur trioxide and re-using it in a circulation step for ufacture of hydroxy aromatics from aromatic sulphonic the production of hydroxy aromatics, whereby acids with sodium hydroxide, namely sulphur trioxide a... sodium sulfite is converted into sodium chloride 35 and sodium hydroxide. and zinc sulfite by means of zinc chloride, The process of this invention for the conversion of b. Zinc sulfite is converted into zinc oxide and sulphur sodium sulfite is thus combined with the well-known dioxide by heating and the latter is processed into process for the production of hydroxy aromatics from sulphur trioxide by oxidation, aromatic sulphuric acids and sodium hydroxide in the c. sodium chloride is converted by means of ammo 40 form of a circulation process in such a way that the nium bicarbonate in order to form ammonium sodium sulfite obtained as a by-product in the produc chloride and sodium bicarbonate, , tion of hydroxy aromatics is converted according to d. Zinc oxide with the ammonium chloride obtained this process into the initial products sulphur dioxide in (c) is converted into zinc chloride in order to and sulphur trioxide and alkali hydroxide respectively recover the zinc chloride consumed in the conver 45 required for the production of the hydroxy aromatics. sion of sodium sulfite, . , , .. Details of this invention are given in the below de e. the ammonia liberated in (d) is used for the forma scription of illustrative examples to which, however, tion of ammonium bicarbonate, and the invention is not limited. f. the sodium bicarbonate is processed into sodium 50 EXAMPLE carbonate and carbon dioxide by heating, and so An about 15-20% aqueous solution of sodium sulfite dium carbonate is processed into sodium hydroxide from a melt of sodium hydroxide and aryl sulphonic by means of calcium oxide. t acid is mixed with zinc chloride. The process of the present invention is carried out in sodium sulfite 126 kilos the form of a circulation process and has the advantage 55 water 500 kilos that the reactants required for the different, necessary zinc chloride 36 kilos chemical conversions are reformed in the course of the The conversion takes place at 25-30°C. The hereby single steps of the process and the resulting by-products practically quantitatively obtained 145 kgs zinc sulfite are consumed again so that after completion of a pro are separated from the about 19% sodium chloride cess cycle no by-products have to be removed. 60 solution. By heating zinc sulfite in usual manner, 64 kgs The conversion of zinc oxide with ammonium chlo sulphur dioxide are liberated and 81.5 kgs zinc oxide ride into zinc chloride and ammonia is practically are obtained. quantitative. Moreover in the conversion of sodium Converting the sodium chloride solution with ammo sulfite according to the present invention exactly those nium bicarbonate into sodium carbonate and further materials are formed or may be converted into such 65 into sodium hydroxide according to the Solvay process, without any particular problems, which are required the ammonium chloride formed during this process will for the production of hydroxy aromatics from aromatic be left. Zinc oxide, together with ammonium chloride, sulphonic acids and sodium hydroxide. will give zinc chloride and ammonia. Whereas ammo 3,929,964 3 4 nia is recirculated for the conversion of sodium chlo sulphuric acid or sulphur trioxide and subsequent con ride, zinc chloride is reused for conversion. version by means of sodium hydroxide. This example clearly proves that by means of zinc The following is added: chloride alkali sulfite may be converted into alkali hydroxide and sulphur dioxide - the latter will give the 1.9 moles = 258 grs ZnCl2) reaction is complete after required sulphur trioxide without causing any troubles Water 30 minutes at about 20°C - and no by-products are obtained which could be re moved only with great difficulties due to the pollution Composition of the combined solution: laws. 10 By this fact the process of the present invention com 1.8 moles = 260 grs ZnSO pares favourably to the Solvay process during which 3.6 moles = 211 grs NaCl 0.1 moles = 14 grs ZnCl calcium chloride in quantities equivalent to those of the 0.1 moles = 14 grs NaSO converted sodium chloride are obtained and which 0.1 moles = 13 grs NaSOa have been removed into waters in the past and caused 4 grs phenolic substances considerable pollution. 15 1, 20 grs water Below are the chemical conversions in the form of l,636 grs chemical reaction equations obtained during the pro cess of example 1: the insoluble ZnSO is filtered off and washed with a 1. NaSOa - ZnCl2 = 2 NaCl -- ZnSO part of the distillate to be recovered later until it is 2.
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