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Is Isszeusall Q Feb. 21, 1956 H. W. RAHN 2,735,750 METHOD OF REDUCING THE CHLORATE CONTENT OF AQUEOUS ALKALI METAL HYDROXIDE WHICH CONTAINS CHLORATE Filed March ll, 1950 N is isszeusall Q f W i N Snipentor M72/wey Maaza/M 66 &/32 - Cittorney 2,735,750 United States Patent Office Patented Feb. 21, 1956 1. 2 lysts include the metals of the eighth group of the periodic system, for example, palladium, cobalt, nickel, ruthenium, 2,735,750 osmium, rhodium, iridium and platinum. These metals METHOD OF REDUCING THE CHILORATE CON in use, however, tend to become coated with nickel which TENT OF AOUEOUS...ALKALE METAL HYDROX is deposited from the alkali metal solution which gen DE WHICHCONTAINS CHLORATE erally contains nickel, and thus it appears that after an Henry W. Rahn, Corpus Christi, Tex assignor to Co lumbia-Southern Chemical Corporation, a corporation appreciable period of operation, with such solutions, nickel of Delaware . is present as an operative catalyst. 0 The process may be conducted simply by pumping hy Application March 11, 1950, Serial No. 149,043 drogen into a pool of aqueous caustic soda solution con taining chlorate, thereby to establish a superatmospheric 8 Claims. (C. 23-184) pressure, and heating the solution. The process also may be conducted in a continuous manner by pumping hy This invention relates to the removal of chlorate and 5 drogen into a pressure reactor, continuously introducing metallic impurities from alkali metal hydroxide. aqueous caustic soda containing chlorate in an upper or Alkali metal hydroxides as produced by some procedures lower portion of the reactor, and withdrawing purified may, and commonly do, contain small amounts of chlorate, caustic soda solution from the other end of the reactor. presumably in the form of chlorate of the alkali metal. The accompanying drawing diagrammatically illus Such chlorate appears, for example, in aqueous solutions 20 trates an embodiment of the invention in which the hy of sodium and potassium hydroxides produced by elec drogen treatment is effected in a continuous manner. As trolysis of the corresponding chlorides in conventional illustrated in this drawing, aqueous sodium hydroxide types of diaphragm cells. Such chlorate is formed, as is solution, containing for example approximately 50 per known, as a result of electrolytic cell reactions. The 25 cent by weight of NaOH and 0.1 to 0.2 percent by weight presence of this chlorate impurity is decidedly objection of chlorate, on the anhydrous basis, is supplied through able. One reason is that its presence in the amounts nor line to heat exchanger 5 by means of a pressure pump 3 mally encountered precludes the use of the hydroxide in which delivers the caustic soda solution to the heat ex the rayon industry. Furthermore, experience has shown changer against an elevated pressure, for example, 260 that chlorate present in aqueous alkali hydroxide is re 30 pounds gauge per square inch. This caustic solution passes sponsible for severe corrosion of iron and nickel equip through the heat exchanger 5 where it is heated to a suit ment used for concentration or storing the solutions. Con able temperature, for example, 180 F., and thereafter is sequently, the concentrated or solid caustic becomes con delivered through line 7 to a pre-hydrogenator 9. taminated with undesired iron or nickel compounds that Gaseous hydrogen is delivered through line 11 to a com may render it off-color and militate against its use for cer 35 pressor 13 and thence through lines 5 and 17 to the pre tain purposes. Also, such attack of concentrating equip hydrogenator. ment increases the production cost of such hydroxides due to the necessity for repair or replacement of equipment The pre-hydrogenator may be of any convenient con that would be unnecessary if the material were chlorate struction which will facilitate intimate contact between free. Metallic impurities also are common in caustic soda 40 the hydrogen and the aqueous caustic in order to permit solutions and, where present in excessive amounts, must rapid saturation of the aqueous caustic. Suitably, it may be removed, comprise a cylinder capable of withstanding the pressures According to this invention, I have discovered that utilized, packed with conventional packing, for example, chlorate may be removed from alkali metal hydroxide % inch graphite Raschig rings. The caustic soda solution solutions by contacting an aqueous solution, preferably and the hydrogen are intimately mixed in the pre-hydro containing not substantially in excess of 75 percent by genator and thereafter pass through line 19 to a second weight of alkali metal hydroxide, with atomic or molecu heat exchanger 2. The hydrogen-caustic soda solution lar hydrogen pressure and a temperature in excess of 125 is passed in heat-exchange relationship to dechlorated C. and preferably at a superatmospheric pressure. I have 50 caustic soda in counter-current flow which is supplied to found that by such treatment of aqueous alkali metal the heat exchanger 2i through line 23 coming from re hydroxide solutions which contain in excess of 0.01 per actor 25. The hydrogen-sodium hydroxide solution ema cent by weight of chlorate, based upon the weight of nates from heat exchanger 2 at an elevated temperature, alkali metal hydroxide in solution, the chlorate may be for example, 290 F., and is delivered to heater 27 through largely or even completely removed within a relatively 55 a spool piece 29 which connects each tube of the heat short period of treatment. I have further found that exchanger 21 with a tube of the heater 27. Heater 27 color normally present in such electrolytic caustic is ap is heated by convenient means, such as steam, which preciably improved by this process. enters the shell of the heater through line 31, condensate The process preferably is conducted in the presence 60 being discharged through line 33. The hydrogen-caustic of a hydrogenation catalyst. However, introduction of soda solution is further heated during passage through catalyst is not absolutely necessary since, in most cases, this heater, and ultimately flows through line 35 to the alkali metal hydroxides contain impurities, notably nickel, top of reactor 25. in small concentrations, and where the alkali metal hy The reactor 25 is of conventional construction, being an droxide is subjected to the hydrogenation treatment in 65 elongated cylinder packed with a suitable packing, for ex the presence of a large solid surface area, metallic nickel ample, nickel Raschig rings. Both the hydrogen and the tends to deposit from the solution upon the surface and hydrogen-caustic soda solution are supplied to the upper thus tends to catalyze further hydrogenation. Hence, the portion of the tower and the solution allowed to trickle reaction may be initiated without recourse to catalyst, if 70 or percolate through the packing downwardly in a hy desired. Other catalysts which are capable of use in cata drogen atmosphere to the bottom of the tower where lytic hydrogenation operations may be used. Such cata the caustic soda collects as a pool. The height of the 2,785,760 3. -- 4 column and the rate of downward flow are adjusted so The following table sets out data which were obtained that the caustic soda solution remains in the tower for in this manner: a substantial period of time, for example, 2 to 30 min Table I lates. Hydrogen Pressure-150 pounds per Square inch. Treated caustic soda which has been dechlorated col 5 Total Pressure-Autogenous pressure of system. lects at the bottom of the reactor. This solution is with Initial drawn through line -23 and is passed in heat-exchange NaOH Chlorate relationship with incoming hydrogen-caustic soda solution Concen- Concen- Time of Percent Temperature of tration, tration, Treat- of into exchanger 21, as has been previously described. Fol Treatment ( C.) Percent Percent by ment Chlorate O by weight based (Hours) Removed lowing this heat-exchange operation, the treated sodium weight on solids hydroxide solution is withdrawn from the heat exchanger in solution 21 through line 41 and is delivered to heat exchanger 5 where it is cooled to approximately 210 F. by heat 50.4 0.066 1.0 0 50.4 0.066 1.0 62 exchange with incoming caustic soda solution, as previ 50.4 0,066 0.5 00 50.4 0.066 0,75 00 ously described. Thereafter, the solution is passed through 50.4 0.066 2.0 50 line 43, through the pressure release valve 45 to reduce the 11.2 0.25 .0 40 11.2 0.25 1.0 22 pressure on the caustic soda solution to atmospheric, 29.9 0.22 1.0 25 7.9 26.9 1.0 80-00 thence through line 47 to the top of a stripping column 69.1 0.085 1.0 56 49 where it flows in countercurrent contact with a stream 69. 0.085 1.75 100 of air introduced at the bottom of the column through 92.1 0,105 0.5 33 line 51. The stripped and purified caustic soda solution is withdrawn from the bottom of the stripper column From the above table, it will be apparent that the rate through line 53 and is delivered to storage. Air rising of removal of chlorate is materially affected by tempera through the column strips the hydrogen from the caustic ture. For example, notwithstanding the fact that the hy soda solution and is vented through line 55 to the atmos drogen pressure was 150 pounds per square inch, no de phere or to other suitable means for discharge of the tectable amount of chlorate was removed at 30° C. from a resulting air-hydrogen mixture.
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