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United States Patent Office 2,750,290 United States Patent Office Patented June 12, 1956 2 the pulping phase of the cycle, thereby obviating the need for substantial storage facilities to contain the re 2,750,290 generated semi-chemical pulping liquor. RECOVERY OF COOKING LIQUOR FROM Another object of the present invention is to provide a SPENT SEM -CHEMICAL PULPNG LIQUORS method for the regeneration of semi-chemical pulping Etagege W. Schoefai, Kronenwetter, Wis, assignor, by liquor, wherein the calcium alkalies recovered with the Kaesare assig nets, to Stering. Drug ac, New York, sodium sulfite can be re-introduced and utilized in the N.Y., a corporation of New York regeneration procedure. No Drawing. Application February 21, 1952, An additional object of the present invention is to pro 10 vide a method for the regeneration of cooking liquor in Serial No. 272,719 high yield from spent semi-chemical pulp liquor, wherein 5 Clains. (C. 92-2) the organic and inorganic materials are substantially com pletely oxidized and converted to usable cooking liquor without the necessity of employing smelting or coking The present invention relates to the semi-chemical l5. procedures. pulping of wood and is more particularly concerned with A further object of the present invention is to provide an improved cycle for the regeneration of sodium sulfite a method for the recovery of semi-chemical pulping (Na2SO3) cooking liquor from spent semi-chemical pulp liquor that insures a continuous supply of regenerated liquors. cooking liquor that can immediately be utilized in the The semi-chemical procedures customarily involve the 20 pulping phase of the semi-chemical pulping cycle. puping with buffered solutions of sodium sulfite. Acid, Other objects of the present invention will be apparent neutral, or alkaline sodium sulfite solutions buffered with to one skilled in the art to which this invention pertains. sodium carbonate, sodium hydroxide or sodium bicarbon The novel process of the present invention is directed ate are representative semi-chemical pulping liquors. The to the recovery of sodium sulfite from spent semi-chemical semi-chemical pulping process results in superior yields pulp liquor and comprises the steps of oxidizing Sub of wood pulp of improved quality and finds applicability stantially completely the said liquor while maintained to a variety of wood materials which cannot be success under the vapor pressure of the reaction mixture and fully cooked by the conventional calcium bisulfite cooking substantially in the liquid phase in a reaction Zone, in acid or other sulfite or sulfate procedure. troducing sulfur dioxide (SO2) and a calcium alkali into However, no technically operative means have been 30 the sodium-containing concentrate from said reaction discovered for the economic reclamation of the sodium zone, separating the calcium sulfate thus precipitated, sulfite cooking liquor from the spent semi-chemical pulp treating the resulting filtrate with a calcium alkali, and liquor. Conventionally the alkali regeneration has been returning the sodium sulfite (Na2SO3) so-formed to the accomplished by concentration of the waste liquor, fol pulping process and the calcium sulfite so-formed to the lowed by a smelting or cooking process in which the 35 said sodium-containing concentrate. In the aqueous, sodium sulfate and sodium sulfite are converted primarily liquid-phase, flameless oxidation of the spent pulp liquor, to sodiuim sulfide (Na2S) and sodium carbonate the inorganic salts are changed to their highest states of (Na2CO3). The generated hydrogen sulfide is expelled oxidation and the sulfurous materials are substantially with carbon dioxide and subsequent treatment with a completely converted into sodium sulfate (Na2SO4), mixture of carbon dioxide, and sulfur dioxide is employed 40 virtually all of the remaining sodium ion being converted to depress the formation of elemental sulfur and thio to sodium carbonate (Na2CO3). The concentration of sulfate or ploythionate salts. The hydrogen sulfide (H2S) the liquor during the oxidation step enhances the Subse is then converted to sulfur dioxide and the reclaimed quent successive conversion of the sodium sulfate to cooking liquor formed from the sodium carbonate and sodium bisulfite and thence to the desired sodium Sufite. sulfur dioxide, eliminating sodium, thiosulfate (Na2S2O3) The amounts of sulfur lost from the system as calcium formation. Maximum yields of the recovered sodium sulfate are at the expense of economically reclaiming Sub ion of slightly over seventy percent have been reported, stantially all of the sodium ion. Careful regulation of arge soda, losses being incurred during the Smelting or the addition of calcium alkalies in the conversion of coking phase of the recovery process. To date, no simple sodium bisulfite to sodium sulfite is productive of an procedure for the regeneration of the semi-chemical pulp 50 already buffered regenerated cooking liquor having the ing liquor (Na2SO3) has been demonstrated to be eco desired pH in accord with the precise type of the semi nomically feasible. chemical pulping process being conducted. Therefore, it is an object of the present invention to The process of the present invention has utility in provide a simple and economical method for the recovery the economical regeneration of the valuable sodium Sul of cooking liquor from the semi-chemical pulp waste fite pulping liquor from the spent semi-chemical pulp liquors in good yields. liquor by a procedure wherein the recovered cooking It is another object of the present invention to provide liquor is immediately recycled to the pulping process, a method for the substantially complete recovery and thereby permitting a virtually continuous pulping opera regeneration of the sodium from spent semi-chemical tion in which the overall sodium loss is small. Recovery pulp liquor. 60 of a small amount of the sodium ion as sodium hydroxide, It is still a further object of the present invention to associated with the sodium sulfite, enables the buffering provide a process for the recovery of sodium sulfite cook action of the sodium hydroxide to be advantageously ing liquor from spent semi-chemical pulp liquor by employed in the regenerated cooking liquor. Useful aqueous, liquid phase, flameless oxidation of the spent amounts of the calcium sulfite (CaSO3) formed in the semi-chemical pulp liquor and conversion of the thus 65 liming of the sodium bisulfite are returned to the phase formed sodium salts in good yield to sodium sulfite of the cycle wherein the sodium sulfate (Na2SO4) is (Na2SO3) and sodium hydroxide (NaOH). reacted with calcium bisulfite (Ca(HSO3)2), produced Another object of the present invention is to provide a in situ. The SO4 ion is eliminated as calcium sulfate, method for the regeneration of the spent semi-chemical which under, controlled roasting conditions yields the pulp liquor wherein the cooking liquor is continuously necessary sulfur dioxide employed in the treatment of recovered from the waste pulp liquor in a properly sodium-containing concentrate obtained by oxidation of buffered sodium sulfite 'solution ready to be returned to the waste liquors. 2,750,290 3 4 In carrying out the process of the present invention, a to the sodium-containing concentrate or added by form starting spent liquor or effluent, resulting from the semi ing calcium bisulfite in situ by reacting sulfur dioxide chemical pulping of soft or hard Woods, or mixtures with a calcium alkali such as calcium carbonate, calcium thereof, with acid, neutral, or alkaline sodium sulfite in oxide, calcium hydroxide, calcium sulfite (CaSO3) and the presence of sodium carbonate, sodium hydroxide or the like in the presence of water. The in situ prepara sodium bicarbonate, and even in the presence of Some tion of the calcium bisulfite is preferred since the calcium sodium sulfate and sodium thiosulfate, is oxidized. Any sulfite produced as a by-product in the Subsequent liming waste liquor or effluent wherein substantial amounts of of the sodium bisulfite can be continuously recycled into sodium sulfite have been employed and are present per the system at this point and admixed with the continu se or in the form of sodium sulfate or sodium thiosulfate 10 ous flow of sulfur dioxide to form the requisite calcium is an appropriate starting material from which the desired bisulfite reagent. The calcium bisulfite reaction step is sodium sulfite can be regenerated according to the process generally conducted in a closed system in order to re of the present invention. duce corrosion of the equipment to a minimum. The In substantially completely oxidizing the spent semi reaction mixture comprising the sodium-containing con chemical pulp liquor, the necessary apparatus comprises 5 centrate and the added calcium alkali is maintained at a pump for continuously charging a reactor with Spent about room temperature or slightly above, temperatures semi-chemical pulp liquor, an air compressor, a tower of 12-25 degrees centigrade being preferred, and the reactor provided with means therein to remove periodi preferred sulfur dioxide gas introduced into the system cally any precipitate formed therein, and a flash chamber over a period of one or more hours. The course of the to receive the oxidized residual spent semi-chemical pulp 20 reaction and degree of completion thereof can be gauged liquor from the reactor. by employing a sufficient analytical control, e. g., a in initiating the oxidation phase, the spent semi-chemi carbon dioxide absorption tube, to avoid the use of an cal pulp liquor is pumped into the reactor under pressure excess of sulfur dioxide. The pH of the sodium bi of from about 200 to 2000 pounds per square inch, the sulfite solution is controlled in part by the amount of preferred pressure being that which is sufficient to main 25 sulfur dioxide utilized in the conversion of sodium sulfate tain substantially all of the waste effluent in the liquid to sodium bisulfite and is preferably less than five, the phase.
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