H. D, GBBS, PROCESS OF MAKNG ALUMNUM CHL ORDE, APPLICATION FILE5 MAY 19, 1921, 422,560. Patented July 11, 1922.

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AA 6/66s, Invenfor fy /s affortney égy E.ARRY D. GIBES, OF PENINS GROVE, NEW SERSEY, ASSIGINo.3. To E. z. Du song SECTEs & COVERANT, OS WILENGTOIT, DEAWARE, A. COR,Rosa.Also, og

5,422,560. Speciication of Letters eatent. Pat eInted July 15, i922. 3:ay 29, 1922. Serial No. 478,843. To all whom it may concern: come very high and therefore it, is possible Be it known that I, HARRY D. GIBBs, 8, to mainufacture aluminium chloride in an citizen of the United States, and a resident iron vessel of the nature of an autoclave of Penns Grove, in the county of Salem and wherein the pressure may rise to may at State of New Jersey, have invented a certain InoSpheres consistent with the strengths of 5 new and useful Process of Making Alumi the iron or steel vessel. un. Chloride, of which the following is a I have also discovered that aluminium specification. chloride is soluble in liquid chlorine, probe This invention relates to the imarifacture bly with the production of a heretofore un of aluminum chloride and comprises a proc described compound consisting of aluminium ess of producing this substance by effecting chloride in combination with chlorine. This a reaction between aluminum and liquid Solution of aluminum chloride in liquid chlo chlorine. rine constitutes a new intermediate product. Heretofore, aiuzminum cihloride has been My new process may be illustrated by the 25 manufactured in several different ways, the following example: Metallic aluminuin in most important of which are: (1) by causing the form of sheets or scrap is placed in a chlorine gas to react with metallic aiuminum vessel which may be made gas-tight, and an at high temperatures; and (2) by bringing excess of liquid chlorine is then introduced. about an interaction between bauxite or The reaction, which is exothermic, begins at 20 alumina, carbon, and chlorine gas. Once and continues rapidly until all the The first of these old processes possesses aluminum has combined with chlorine to the disadvantages that the temperatures re form AlCla. Shortly after the reaction has quired are very high, and the excessive ac started, the heat generated brings the liquid tion of the chemicals upon the apparatus re chlorine to the boiling point. The chlorine 25 quires frequent and expensive replacements. vapors formed may be allowed to pass into a Moreover, the aluminium melts and thus reflux condenser cooled by chilled brine or 80 presents only a small surface to the action of other cooling medium. In some cases it is the chlorine gas thus slowing the speed of desirable to cool the vessel in which the reac the reaction. The aluminium chloride dis tion is taking place. The mixture of alumi 30 tils out of the apparatus and is condensed, a num, and chlorine should preferably be rather difficult and troublesome operation. stirred as the reaction proceeds. If suffi 85 The second of the above mentioned old cient cooling is provided for, it is not neces processes presents many of the same disad sary that the pressure in the apparatus rise. vantages enumerated above, in that exces above five atmospheres; however, it is no dis 35 sive action of the reagents necessitates fre advantage to allow the pressure and the tem (quent and expensive replacements. perature to rise to higher limits consistent 90 i have discovered that aluminum will com with the strength of the apparatus. if the bine with chlorine at relatively low tempera reaction proceeds in too violent a manner, tures, and that the reaction may be most ad the liquid chlorine may be introduced in 40 vantageously effected by bringing the alu smaller quantities or the cooling may be in minum into contact with liquid chlorine. I creased. 95 have found that the reaction between these Upon completion of the reaction the un two elements takes place rapidly at the changed chlorine is distilled off and can be boiling point of chlorine at atmospheric condensed and used again with new batches pressure; namely, approximately -33°. of aluminum. There is left aluminium With elevated temperatures, the reaction is chloride in a dry state in the form of a more more rapid. At the elevated temperatures, or less granular powder in the most active it is necessary to form the reaction in a form that this compound can be used for the closed vessel, thus taking advantage of the various organic condensations or for the 50 increased pressure of the chlorine to raise the cracking of petroleum or other uses. boiling point of the liquid chlorine and thus The new process may be carried out in OS keep it in the liquid state. The reaction be various forms of apparatus, one form being tween iron or steel and liquid chlorine does illustrated in the accompanying drawings, not take place until the temperatures be in which Figure 1 shows a vertical section 2 1422,560 through the center of the autoclave, and sure, I may under certain circumstances op 60 Figure 2 shows a plan view of the cover of erate at a temperature substantially below the autoclave. the boiling point of the liquid chlorine at The apparatus comprises an autoclave 4 any given pressure Cooling the reaction having around its upper edge an outwardly mass to a temperature below the boiling extending flange 5 provided at regular inter point of liquid chlorine is sometimes desir 65 vals with recesses adapted to register with able for the purpose of moderating the re corresponding recesses 6 in the edge of the action in case it becomes too violent. autoclaye cover 7, the recesses being designed I claim :- 0. to receive bolts 8 for holding the cover in 1. The process of producing aluminum place. chloride which comprises bringing aluminum 70 The cover 7 has a hole through the center into contact with liquid chlorine. through which extends a shaft 9 carrying 2. The process of producing aluminum stirring arms 10. The end of a reflux con chloride which comprises subjecting alumi 15 denser 11 extends through the cover, the lat num to the action of liquid chlorine at about ter being also provided with a hole 12 for the boiling point of the latter. 75 the introduction of chlorine from a supply 3. The process of producing aluminum tank 13, and with a filling hole 14 through chloride which comprises subjecting alumi which the aluminum may be introduced. A num to the action of liquid chlorine at at 20 thermometer well is indicated at 15. pressure substantially above atmospheric The condenser is provided with a jacket 16 pressure. 80 for the reception of chilled brine or cold 4. The process of producing aluminum water. The upper end of the condenser is chloride which comprises subjecting alumi in communication with a pressure gauge 17. num to the action of liquid chlorine at about 25 A needle valve 18 is located beyond the pres its boiling point and under a pressue sub Sure gauge connection. The supply of chlo stantially above atmospheric pressure. 85 rine may be regulated by a valve 19. 5. The process of producing aluminum The operation in this apparatus is as fol chloride which comprises subjecting alumi lows: w num to the action of liquid chlorine at about 30 The required quantity of aluminium is its boiling point and under a pressure of placed in the autoclave 4, through the filling about 5 atmospheres above atmospheric pres 90 hole 14; this hole is then closed and the liquid Ste. :: chlorine in excess is run in from the chlorine 6. The process of producing aluminum cylinder 13, by opening the valve 19. The chloride which comprises subjecting alumi 35 heat of the reaction causes the chlorine to num to the action of liquid chlorine, the boil and the vapors are condensed in the con amount of liquid chlorine present being in 95 denser 11 which is cooled preferably, by excess of that theoretically required, allow chilled brine circulating in the jacket 16, ing the reaction to proceed until substanti and the condensed vapors are returned to the ally all the aluminum has been converted into 40 autoclave in the form of liquid. If the pres aluminum chloride, and then distilling off sure becomes too great, as shown by the gauge the excess chlorine. 00 17, it may be released by opening the valve 7. The process of producing aluminum 18. The autoclave 4 may also be cooled by chloride which comprises subjecting alumi surrounding it with chilled brine and the num to the action of chlorine at a tempera 45 contents may be agitated by rotating the stir ture below 0° C. ring shaft 9. 8. The process of producing aluminum 05 in completion of the reaction, the chlorine chloride which comprises immersing alumi may be distilled out of the autoclave, and the num in liquid chlorine, allowing the liquid dry aluminium chloride removed; or the to boil and the vapors to pass into a reflux 50 aluminium chloride may be used in the auto condenser, and maintaining the absolute clave 4 by adding other chemicals suitable pressure below 10 atmospheres. 10 for the production of various reactions with 9. As a new composition of matter a solu aluminium chloride. tion of aluminum chloride in liquid chlorine. Although I prefer to operate in such a wav. 10. As a new composition of matter a solu 65 that the aluminum will react with liquid tion of 1 part aluminum chloride in 1A parts chlorine at the latter's boiling point, in order liquid chlorine. 5 to get the benefit of the maximum tempera In testimony whereof I affix my signature. ture consonant with maintaining the chlorine in the liquid condition and under a safe pres HARRY D. GIBBS.