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United States Patent Office Patented Aug 3,145,079 United States Patent Office Patented Aug. 18, 1964 2 3,45,079 The carbon used in the process of this invention can PROCESS FOR THE PREPARATION OF PJR-FED be located in any convenient vessel, most preferably in HYDRC:{SEN BROMIDE GAS BY THE USE OF a column or tower bed in conventional equipment. The ACTWATED CARBON AS CATALYST tower or column is preferably located immediately fol Max L. Harbagh, New Shrewsbury, N.J., assignor to E. lowing the hydrogen bromide gas generator or reactor in da Poat de Nemours and Company, Willinington, Dei, such a manner that any drip back or condensate from a corporation of Delaware the column is returned to the reactor. No Drawing. Fied Oct. 31, 1961, Ser. No. 48,805 With reference to an activated charcoal column oper El Cain. (C. 23-354) ation, the inlet temperature of the column approaches 10 the operating temperature of the hydrogen bromide gas This invention relates to the preparation of hydrogen generating reactor, which is within the range of 100° C. bromide. to 160° C. The heat effects in the column are negligible. Prior art processes of preparing hydrogen bromide gas Thus, a gradual progressive cooling due to natural radia by reducing bromine with sulfur in the presence of water tion through walls to the atmosphere occurs during pas have been found to produce a gaseous product containing 15 Sage of the hydrogen bromide gas stream through the sulfurous impurities and unreacted bromine. These sul column so that outlet temperature can be as low as furous impurities have not all been completely identified, ambient atmospheric temperature or approach the inlet but include various partially oxidized and volatile com temperature, depending upon the volume of throughput. pounds of Sulfur, oxygen and bromine, formed in the re The inlet gas temperature may reasonably be about 100' duction process. These sulfurous impurities, upon ad 20 C. to 135 C. with the appropriate temperature gradi Sorption in water and Subsequent oxidation, are analyzed ent through the length of the column. Ambient tem as Stilfates. It is believed that among these impurities are peratures can range to as low as about 25 C. In gen sulfur dioxide and thionyl bromide (SOBr.). eral, the upper temperature of the carbon bed will not Prior art attempts to remove these sulfur impurities rise above the temperature of constant boiling hydro from the gaseous hydrogen bromide stream by dissolu 25 bromic acid, i.e., about 126 C. tion in a solvent have not proved satisfactory since the The carbon bed is maintained essentially at atmospheric method is costly and not sufficiently efficient. pressures, i.e., about 1 to 2 inches of water pressure. The According to the present invention, these impurities pressure of the column is not a factor in this step. If can be removed from gaseous hydrogen bromide which 30 preferred, it is only necessary to use sufficient pressure is made by reducing bromine with sulfur in the presence of to promote the flow of gas through the column and Water. The invention comprises the improvement of through the subsequent equipment. In general, satis passing the impure hydrogen bromine gas through a car factory inlet pressures of about 1 to 2 inches of water bon-packed bed or column, and then collecting the exclusive of the back pressure of subsequent adsorption purified hydrogen bromide gas. 35 equipment are suitable. The constituency of the hydrogen bromide stream Column or tower design can be conventional. A being purified will ordinarily comprise not more than column length over diameter ratio in the range of 1.5 to about 2%, by weight, of sulfurous impurities, based on 2 is preferred. The design gas velocity is in the range of total sulfur present, not more than 2%, by weight, of 0.5 foot per minute to 2.0 feet per minute. The gas bromine, and at least two moles of water for each mole 40 flow rates per unit volume of packing range from about of Sulfurous impurity calculated as SO2. These com 0.2 to 1.0 cubic foot of gas per minute per cubic foot ponents should be present in stoichiometric proportions. of packing. The gas residence time in reaction zone is in Preparation of a hydrogen bromide stream of this con the range from about 1 to 10 minutes. stituency is described in detail below. 45 As stated above, the amount of water in the hydrogen The carbon used according to the present invention bromide stream being purified should be at least 2 moles is preferably that known as activated charcoal. The car of water for each mole of sulfurous impurity calculated bon apparently catalyzes a reaction in which the sulful as SO3. Above this limit, the water content can be per rolls impurities and certain bromine compounds in the mitted to vary over wide limits. hydrogen bromide gas stream react to form sulfuric acid 50 The maximum limit of water content is that at which and hydrobromic acid, with the result that the gas leav is formed the equivalent constant boiling composition of ing the carbon is essentially all hydrogen bromide, con hydrobromic acid, i.e., 48% HBr. In other words, the taining only water vapor as an undesired component. amount of water present should be less than 52 parts of Since the carbon is used as a catalyst rather than an ad water per 48 parts of hydrogen bromide. Otherwise, if sorptive purifier, it can be used for extended periods the column or tower temperatures are less than the boiling without treatment to remove impurities. point of constant boiling hydrobromic acid (about 126 The water content of the final product can be sub C.), equivalent materials will condense and reflux back sequently reduced to desired limits by any suitable means, to the tower or column. Such as by ordinary refrigeration, or by passing the prod 60 Since it is highly desirable according to this invention luct stream through a conventional cold trap operated, for to produce an anhydrous gas as a final product, the example at reflux. An alternative drying method, such amount of water permitted to go into the column or tower as the use of a conventional desiccant bed, can also be containing the carbon is preferably held towards the used. minimum by means of controlling the water feed to the 3,145,0 79 3 4. system. The amount of water entering the system can a generator consisting of a 2-liter standard laboratory conveniently be controlled by adjustment of the concen 4-necked reaction flash arranged with an agitator, drop tration of the sulfuric acid in the preparation of the ping funnel, thermometer, and gas outlet. The gas out hydrogen bromide, as will be explained more fully below. let leads to a vertical column two inches in diameter by The sulfuric acid which forms in the carbon bed as 5 25 inches high packed with activated charcoal, and ar a result of the catalytic reaction of the residual bromine ranged for reflux of any drip-back to the reaction flask. and sulfur compounds, collects on the surfaces of the The effluent gas from the charcoal column is led to a carbon particles to form a condensate which drips back to low temperature condenser also arranged in reflux. The the gas generating reactor as a reflux stream. charcoal column inlet temperature is about 125 C. to In general, the purified hydrogen bromide gas issuing O 127 C. and the outlet temperature is essentially at room from the carbon-packed bed contains not more than temperature due to radiation cooling. The column input about 0.10 weight percent of sulfurous impurities and not pressure is about 1 inch of water pressure and the aver more than about 0.10 weight percent of elemental age residence time of the hydrogen bromide stream being treated in the charcoal column is about 1 minute. bromine. Over a four-hour continuous operating period, the PREPARATION OF HYDROGEN BROMIDE effluent gas from the activated charcoal column is bro The hydrogen bromine gas stream which is treated with mine-free and contains only about 0.03% to about 0.12% carbon according to the procedures of the present inven Sulfur compounds as sulfur dioxide, as contrasted to tion can as referred to above, be suitably prepared 1.25% free bromine and .95% sulfur compounds before according to conventional procedures. 20 carbon treatment. The product recovery is 98.7%. The impure hydrogen bromide gas is prepared in such a way that the gas contains stoichiometric quantities of Example 2 sulfurous impurities and gaseous bromine, and water The process of Example 1 is repeated, conducting three vapor. A suitable procedure involves stoichiometric feeds intermittent runs for a total of 13.5 operating hours. In of sulfur and bromine to a reaction heel of sulfuric acid, 25 this over-all period, the effluent pure hydrogen bromide maintained at a selected temperature and concentration, gas is bromine-free and contains only about 0.01% to with the reaction occurring to form in major part hydro about 0.09% sulfur dioxide. The chemical yield of gen bromide and in lesser part to form volatile sulfur and bromine to hydrogen bromide is 96.4%. The chemical bromine compounds. When equilibrium conditions have yield of sulfur to sulfuric acid is 100.4%. The weight of been established in the resultant reaction heel, surprisingly, charcoal used is 286 grams. The total weight of bromine the sulfur and bromine compounds which do volatilize to fed is 2,270 grams, equivalent to 168 grams per hour, so in stoichiometric proportions, so that subsequent cata and at a gas Velocity of 2.5 feet per minute in the char lytical reaction to completion of these compounds pro coal column.
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