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United States Patent Office Patented Apr. 9, 1946 2,398,179 UNITED STATES PATENT OFFICE. P MANUFACTURE OF ETHYL CHLoRIDE Eugen Gottfried Galitzenstein, London, and Cyril Woolf, Finchley, London, England, assign ors to The Distillers Company Limited, Edin burg, Scotland, a British company No Drawing. Application March 9, 1944, Serial No. 525,758. In Great Britain December 28, 1942 20 Claims. (CI, 260-652) It is known that ethyl chloride is formed when densed out. The yield of pure ethylchloride, ob potassium or barium salts of ethyl sulphuric acid tained over a period often hours, was 102 grams are treated with hydrogen chloride (Berichte der or 93 per cent of the theory. Deutschen Chemischen Gesellschaft 1878, 11, 1929). In British specification No. 370,211 there Eacample II is described a process in which ethyl chloride is Into a stirred mixture of 220 grams diethylsul produced when ethyl Sulphuric acid is caused to - phate, 36 grams sulphuric acid (98 per cent) and . react with a qieous hydrochloric acid at tempera 6 grams bismuth oxide, dry hydrogen chloride tures exceeding 100° C. and at elevated pressures was introduced at the rate of about 6 grams per Such as 24 atmospheres. w O hour whilst maintaining a temperature of 80° C. We have found that ethyl chloride can be pro in the reaction liquid. The escaping gases were duced Satisfactorily according to the present in washed with water and then with milk of lime, vention by reacting gaseous hydrogen chloride dried with calcium chloride and the ethyl chlo with preformed sulphuric esters of ethyl alcohol ride condensed out. In 20 hours 163 grams of in the presence of a compound of antimony, bis practically pure ethylchloride were collected, the nuth or tin as catalyst at temperatures between yield being 90 per cent of the theory. 40' and iO C. The chlorides, oxides, sulphates or carbonates of antimony, bismuth and tin may Eacample III be used. A stirred mixture of 105 grams diethylsulphate, The reaction between ethyl hydrogen sulphate 20 70 grams sulphuric acid (100 per cent) and 17 and hydrogen chloride proceeds according to the grams anhydrous tin tetrachloride was treated equation: with a stream of about 7 grams per hour of dry hydrogen chloride at a temperature of 98°C. The (1) Cahs.HSO4-HCl=CasCl--H2SO4 escaping vapours were led through a fractionat and can be carried out at normal pressure. 25 ing Column at the top of which a vapour tem Instead of ethyl Sulphuric acid, diethyl Sulphate perature of 13 C. was maintained by means of a can be used. We have found that when ethyl reflux condenser. After washing and drying eth chloride is produced by the interaction of hydro ylchloride was condensed at the rate of 12 grams gen chloride and diethyl sulphate in the presence per hour. of compounds of antimony, bismuth or tin, the 30 It will be inferred from Equations 2 and 1 initiation of the reaction is facilitated by the that on completion of the reaction between the presence of Some free sulphuric acid in the reac esters of sulphuric acid and hydrogen chloride, tion mixture at the Commencement of the reac free sulphuric acid is present together with the tion. The probable function of this free sul metal compounds. We have found that the spent phuric acid is to cause the formation of ethyl 35 liquids resulting from the reaction between ethyl sulphuric acid according to the equattion: . sulphuricesters and hydrogen chloride have the power of absorbing ethylene thus reforming the original sulphuric acid esters. The reformed es The following examples illustrate the process ters are capable of reacting again with hydrogen of the invention as a batch process: 40 chloride to produce ethylchloride without the Eacample I necessity of further addition of compounds of antimony, bismuth and tin. A stirring fiask was charged with 214 grams Accordingly, therefore, our invention includes ethylsulphuric acid. 14 grams of anhydrous an a process for the manufacture of ethyl chloride timony trichloride were added and dry hydrogen 45 from ethylene. The process consists of a number chloride was then introduced at the rate of about of cycles, each cycle comprising two stages. In 8 grams per hour whilst maintaining the liquid the first stage, ethylene is absorbed by sulphuric at a temperature of 90° C. Stirring was con acid. Compounds of antimony, bismuth or tin titled throughout the Operation. The vapours are added to the resulting liquid and the second escaping from the stirring flask consisted of ethyl 50 stage of the process consists in reacting the mix chloride accompanied by Some excess of hydrogen ture with hydrogen chloride to produce ethyl chlo chloride which was removed from the ethyl chlo ride. These two stages comprise the first cycle. ride by Washing with Water and then with Caustic In the first stage of the second cycle, ethylene is soda solution. The vapours of ethyl chloride again absorbed following which, hydrogen chlo were dried with calcium chloride and then Conn 55 ride is again passed through the liquid reaction 2 2,898,179 medium, which still contains the catalyst remain liquid showed an increase in Weight of 47 grams ing from the first cycle, producing ethyl chloride: corresponding to an absorption of 0.9 no of this constitutes the second stage of the second ethylene per mol of sulphuric acid. The ten cycle. Further cycles are the same as the second perature was then raised to 90' C., hydrogen chlo cycle. s ride was introduced and ethylchloride condensed We prefer to carry, out our process in a sub out of the effuent gases. When the production stantially anhydrous medium using sulphuric acid /rate of ethylchloride began to decrease, the hydro of between 100 per cent and 95 percent by Weight. gen chloride stream was stopped, the temperature We have found it to be advantageous in the lowered to 70° C. and ethylene introduced (begin stages of ethylene absorption to introduce ethyl ning a second cycle of Operations) and the ab ene until the concentration of ethyl groups pres sorption of ethylene was continued until an in ent (in the form of the sulphuric esters of ethyl crease in weight of 38 grams had occurred thus alcohol) has reached between 0.7 to 12 mols per again bringing the total amount of ethyl groups mol of sulphuric acid. Such mixtures of diethyl present to 0.9 mol per mol of Sulphuric acid. sulphate, ethylsulphuric acid and sulphuric acid s The Subsequent introduction of hydrogen chloride have been found to be the most suitable for the was carried out at 90° C. Further cycles followed production of ethylchloride. Furthermore we in a way similar to the last cycle. After a Work have found it unnecessary to continue the hy ing time of 150 hours the yield of ethylchloride drogen chloride introduction to the point of com produced based on ethylene absorbed amounted pletion of the reaction: we prefer to stop the flow 20 to 88 per cent of the theory. of hydrogen chloride when the rate of ethylchlo Instead of pure ethylene, gas mixtures contain ride production slackens off. This generally oc ing ethylene, e. g. mixtures of ethylene and paraf curs when the concentration of ethyl groups has fin hydrocarbons; can be used. We have found it fallen to the neighbourhood of 0.25 mol per mol advantageous to employ elevated pressure in the of sulphuric acid present in the reaction medium. 92.5 ethylene absorption stage when using ethylene By leaving some unreacted ethyl groups in the so admixed with other gases. The corresponding lution, the subsequent absorption of ethylene is stages of ethylchloride production may be car enhanced, as is already known from prior British ried out in a separate vessel and at ordinary pres specification No. 221,512. sure. Previous processes (e. g. that described in The following examples illustrate the process of 30 United States specification No. 2,125,284) relating the invention as a Continuous process consisting to the direct reaction between hydrogen chloride of a number of successive cycles. and gas mixtures containing ethylene have proved to be technically unsatisfactory as the presence of Eacaraple IV inert gaseous substances depresses the rate of for A stirring vessel was charged with 180 grams mation of ethylchloride and gives rise to difficul sulphuric acid (98 per cent) and 12 grams an ties in the recovery of the diluted ethylchloride. hydrous bismuth chloride. The contents of the However, the ethylchloride obtained by our proc vessel were stirred and maintained at 70° C. dur ess, is contaminated only with hydrogen chloride, ing the whole operation. Dry ethylene was intro which is readily removed. duced at the rate of 11-12 grams per hour for 4 40 Instead of a stirring vessel, other suitable de hours. The ethylene supply was then cut of and vices can be employed for alternately contacting dry hydrogen chloride introduced at the rate of the liquid reaction medium with ethylene and about 9 grams per hour to start the production of with hydrogen chloride. For instance the two ethylchloride. When the rate of formation of gases may be alternately passed into a coil sys ethylchloride dropped below a figure of 6 grams tem through which the liquid reaction medium is per hour the introduction of hydrogen chloride circulated at high speed with aid of a pump. - was cut off, the passage of ethylene was restarted The experiments on which the present inven and the second and subsequent cycles carried out. tion is based proved that the presence of Con The results of the entire operation are Sun pounds of antimony, bismuth or tin is essential marized in the following table: 50 for the manufacture of ethylchloride from hydro gen chloride and the ethyl esters of sulphuric acid.
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