an nucnuna, or nanoynn-nrnrn, GERMANY, ASSTGNOR T40 ALBERT . . ETER nornayor zunrcu, swrrananann. JPEOUJESS 0h‘ iMANUT'ACTURTNG COMPJLEX HYDROT‘LUORTG ?AlLT. vIla hrag. original application filed July 2e, 19%, Serial No. 7%,545, and in Germany July so, letd Divided. and this application ?led January 28, 1927. Serial No. 164,371. salts according to the invention the, follow This application is a division of my ap plication Serial No. 727,545 ?led duly 22nd, mg equation takes plate 2+ 192d. ' For the manufacture of,hydro?uo-sil_icic h salts there are known only very inconvenlent Sometimes it is advantageous, to ‘work in ' methods, which are not easily carried out presence of an acid, the added acid being on afmanufacturing scale with commercial only a contact substance and small amounts success.- Generallythydro?uoric acid and hy are sufficient. and vhandling of' hydro?uoric acid are ing equation :- till ‘ An example for the manufacture of other dro?uo-silicic acid have to be made ?rst, so 10 that all the di?iculties of the manufacture complex hydro?uoric salts shows the follow ‘ ' brought into ‘the manufacture of hydro?uo ZNaCl + 2BR + Call‘2 (hydrochloric acid) = . silicic. salts, 65 Qhlaldll‘4 + @aCl2 (hydrochloric acid) _ _ This invention comprises a new way of it making directly from its components not\ Hydrochloric acid being contact substance only hydro?uo-silicic salts, but also complex. as above - mentioned. The reaction is also hydro?uoric compounds.’ possible Without acid. _ , i As already stated, in all cases the most lit consists ‘in treating a ?uoric salt with silicon-tetr'a-?uoride in presence of a decom convenieht ?uoride for the starting ?uoride 20 posable salt of the base, which shall be com is ?uorspar, which can be easily and cheaply 70 obtained. ' An insoluble ?uoride is as a rule bined with the hydro?uo-silicic acid. With the complex» salts of ?uorine instead preferable, in so far as the ?uoride is only ofsilicon-?uoride the corresponding ?uor an assisting component in the process. That hydrochloric acid may be used in the ides of other complex forming elements are reaction is shown by the last equation. 25 used. For assisting the formation of these com Chlorides in the form of metalchlorides are pounds the reaction is carried out under favorable as a soluble salt component in the pressure or under pressure and at high tem reaction. But any other salt can be used, perature. Volatile compounds, which re which is decomposable under the conditions so sult fromthe reactions, can be separated by of the process .by the other reaction compo nents. Tn the manufacture of ‘complex ?uorides Furthermore, the process can be carried distillation. ' _ 4 ' out with, solid raw materials or with so little another way is to let the ?uoride of the com llll solvent that, a solution ofthe reagents and'of plex forming element ‘and hydro?uoric acid react upon a salt the corresponding base of The ‘complex hydro?uoric salts are thus which is to form partof the complex com ,wobytained directly from the components by pounds. The acid of this salt is then obtained "at a the compounds formed can not talze plate. ' the process. -' as free acid. ' to hydrouo-silicic salts this new process has ‘1 eat advantages. ‘ I ' ' ' llll The following equation is a type of this * (lo ‘I :. ared with known‘ methods of making, reaction ':— -' _ _~;.The manufacture of the salts is completed inone operation, whereas heretofore the ini - - _hIaUl-l-BFS+HF=NaBTT4+HGl The advantages of'this new process are/in manufacture of hydro?uoric acid'by diss vthis case not so com lete as may be, though I = .‘ ‘ t was necessary, with subsequent sat acid is obtained as y~product. Therefore a: tillatio'n of this ‘acid with silicic acid. The special ways shall be shown, where a ?uoride‘ ' ; .urati p cation-of the process results in a furnishes the ?uorine for the operation. The following is an example for vworlr at saving of time and of machinery. @onceg the manufacture of hydro?uo- ' fl cic. salts, or complex hydro?uoric salts the ffloll may be stated. '_ ' in 2- _ I .. _ %% hg?uoride of calcium are mixed with 117 lrg. chloride of sodium adding to the min e manufacture of hydro?uo-silicie ture water, ‘which has been acidi?ed with‘ llllll 1,685,628 hydrochloric acid. While stirring this mix shall be produced, in the presence of a small ture and heating to a temperature of about ‘amount of acid as contact substance. 40° C. .boro?uoric gas is led in. Soon the 5. Process of manufacturing hydro?uo precipitation of sodium boro?uoride begins. silicic salts, which comprises reacting on The reaction is complete, when 116 kg._boro 40 ?uor-spar with silicon?uoride in presence of ?uoride have been added. Then sodiumboro a chloride and in presence of asmall amount ?uoride is ?ltered and washed with water, of hydrochloric acid as contact substance. which can easily be done. 6. Process of manufacturing complex hy I claim-— , , y _ dro?uoric salts by the reaction of a simple 10 1. Process of manufacturing complex hy ?uorine-compound with the ?uoride of an ele dro?uoric salts, which comprises reacting on ment of the group consisting of silicon and 45 I an alkali earth metal ?uoride with the ?uor~ boron and a salt of the alkali metal whose ide of an element of the group consisting of complex hydro?uoric salt shall be produced, silicon and boron in the presence of a salt of under pressure higher than atmospheric pres the alkali metal whose complex hydro?uoric salt shall be produced. sure. 7. Process of manufacturing complex hy 2. Process of manufacturing complex hy dro?uoric salts by the reaction of a simple dro?uoric salt, which comprises reacting on ?uorine compound with the ?uoride of an 20 an insoluble metal ?uoride with the ?uoride element of the group consistin of silicon and of an element of the group consisting of sili boron,‘ and a salt of the alka i metal Whose con and boron in the presence of a salt of the complex hydro?uoric salt shall be produced, 55 alkali metal whose complex hydro?uoric salt under pressure higher than atmospheric pres shall be produced. ~25 30 ' sure and at a temperature higher than atmos 3. Process of manufacturing complex hy pheric temperature. dro?uoric salt, which comprises reacting on I 8. Process of manufacturing complex hy an insoluble metal ?uoride with the ?uoride dro?uoric salts by reacting on a simple of an element of the group consisting of sili ?uorine compound with the ?uoride of an ele con and boron in the presence of the chloride ment of the group consisting of silicon and of the alkali metal whose complex hydro boron, and a salt of the alkali metal whose ?uoric salt shall be produced. complex hydro?uoric salt shall be produced, 4. Process of manufacturing complex hy working in presence of an amount of solvent dro?uoric salt, which comprises reacting on insufficient for the solution of the reaction an insoluble ?uoride with the ?uoridevof an element of the group consisting of silicon 35 and boron in the presence of a salt of the al kali metal ‘whose complex hydro?uoric salt‘ components. . In testimony ‘whereof I a?ix my signature. DR. MAX BUCHNER 60 65
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