SE128373C1 - - Google Patents

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Publication number
SE128373C1
SE128373C1 SE128373DA SE128373C1 SE 128373 C1 SE128373 C1 SE 128373C1 SE 128373D A SE128373D A SE 128373DA SE 128373 C1 SE128373 C1 SE 128373C1
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Sweden
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ether
solution
bisulfite
naoh
washing
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Swedish (sv)
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Publication of SE128373C1 publication Critical patent/SE128373C1/sv

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  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Description

Uppfinnare: G. Hallie. Inventor: G. Hallie.

Prioritet begard frdn den .0 september 1947 (Nederliinderna). Priority was given to .0 September 1947 (Nederliinderna).

Tekniskt, t. ex. over etylsulfat, framstalld eter kraver raproduktens rening for att erMita kemiskt ren resp. narkoseter. Malin har bland annat foreslagits att tvatta thetern med bisulfitlasning, som innehaller en icke flyktig, vattenblandbar alkohol, I. ex. etylenglykol, varefter produkten tvattas med en natriumhydroxidvattenlosning. For att erhalla narkoseter maste raprodukten aven i farvag tvattas mod en liknande natriumhydroxidlosning. Technically, e.g. over ethyl sulphate, prepared ether requires the purification of the crude product in order to be chemically pure resp. narcotics. Among other things, Malin has been suggested to wash the theater with bisulfite glazing, which contains a non-volatile, water-miscible alcohol, I. ex. ethylene glycol, after which the product is washed with an aqueous sodium hydroxide solution. In order to obtain anesthetic ether, the rap product must also be washed in color against a similar sodium hydroxide solution.

Foreliggande uppfinning hanfor sig till ett forfaringssatt for framstallning av myeket Ten eter, i synnerhet narkoseter, vilket satt bestar dari, att raetern tvattas med en bisulfit innehallande losning pa ett mycket enkelt satt, varigenom tvattningen med natriumhydroxidlosning kan bortfalla. Sattet enligt uppfinningen kannetecknas darav, att pH-vardet av den anvanda bisulfit innehallande lasningen ligger inellan lnA(8)InA() ,2 + 10 ln 2 och 6,3 + 10 ln 2' varvid A(8) betyder den faktor, som visar bisulfitlosningens utspadning i jamforelse med en standardlosning, som framstallts genom inledning av SO, i en 8 %-ig NaOH-losning. The present invention relates to a process for the preparation of a lot of ether, in particular anesthetic ether, which method consists in washing the ether with a bisulfite-containing solution in a very simple manner, whereby the washing with sodium hydroxide solution can be eliminated. The process according to the invention is characterized in that the pH value of the bisulfite-containing weld used is between 1nA (8) InA (), 2 + 10 ln 2 and 6.3 + 10 ln 2 ', where A (8) means the factor shows the dilution of the bisulfite solution in comparison with a standard solution, prepared by initiating SO, in an 8% NaOH solution.

Det har visat sig, att de bisulfit innehallande Idsningarnas koncentration är av starsta betydelse for uppnaendet av goda tvd.ttresultat. Foreliggande uppfinning har bland annat till syfte alt angiva tvattvatskans exakta koncentration. It has been shown that the concentration of the bisulfites containing the icings is of the utmost importance for the attainment of good TV results. The object of the present invention is, inter alia, to indicate the exact concentration of the wash water liquid.

Det antages, att den bisulf it innehallande losningen har framstallts genom att neutrallsera en NaOH-lasning medelst SO, och att S0,-tillforseln fortsattes en viss tid utover det ogonblick, d alit NaOH har omvandlats i Na,SO„ Slutlosningen innehaller sedan en viss mangd NaHSO, sand tiarierande mangder an- tingen SO, (ILS0a) ochjellerTydligen aro foljande faktorer av betydelse: 1. Lasningens Na0H-koncentration. Givet vis innehaller losningen efter avslutad inledning icke langre fritt Na0H, men vatskans natriumhalt kan av bekvamlighetsskal uttryckas i NaOH. 2. Forhallandet mellan mangderna SO, och NaOH. Det har namligen visat sig, att faktor 1. är av mindre stor betydelse, emedan a.ven nar de bisulfit innehallande losningarna till och med visa stora skillnader i sin NaOH- halt, goda tvatteffekter kumia uppnas. Daremot Or faktor 2. av storsta betydelse och foljaktligen är det lampligt att narmare ing'd harp a. It is assumed that the bisulfite-containing solution has been prepared by neutralizing a NaOH solution by means of SO, and that the SO2 feed was continued for a certain time beyond the moment that NaOH has been converted to Na2 SO2. amount of NaHSO, sand tiering amounts either SO, (ILSO 3) and / or Apparently the following factors are important: 1. The NaOH concentration of the weld. Of course, the solution after completion of the solution no longer contains free NaOH, but the sodium content of the liquid can conveniently be expressed in NaOH. 2. The ratio between the amounts of SO, and NaOH. Namely, it has been shown that factor 1 is of less importance, because even when the bisulfite-containing solutions even show large differences in their NaOH content, good washing effects kumia are achieved. On the other hand, Or factor 2. of the greatest importance and consequently it is appropriate that closer ing'd harp a.

I denna beskrivning och i patentanspraken uttryckes forhallandet SO,:NaOH i pH. Detta Or tvivelsutan lampligt och exakt, emedan det ena sidan an ganska svart aft bestamma eller definiera detta forhallande direkt. Ringa mangder SO, medforas av etern under tvattningen, sâ att pH-matningar aro ett enkelt medel for att reglera tvattvatskans koncentration. A andra sidan innebar SO,-tillforseln en surgoring, som medlar pH-vardets sjunkande, sâ att ett givet pH motsvarar endast ett bestamt forhallande SO, :NaOH. Foljaktligen utgar pH-vardet en korrekt mattstock. For en losning, som innehaller 8 % NaOH (neutraliserat), Oro pH-granserna 5,2 och 6,3. Arbetar man daremot med mera utspadda eller mera koncentrerade losningar an en 8- procentig, uppkommer en svarighet, eftersom en utspadning hOjer pH-vardet, under det att farhallandet So, :NaOH forbliver konstant. Med andra ord stamma vardena for en 8-procentig losning icke for en mera utspadd med samma forhallande SO.,:Na0H. I ett sadant fall maste andra varden angivas och likash i vart fall, dar andra koncentrationer anvandas. Att angiva de korrekta pH-vardena fOr alla losningar samtidigt, kraver en formel, som innehaller ett korrektionsvarde for den forandring, som intrader vid utspadning. Detta korrekturvarde liar experimentellt faststallts. Inledes 1 en 25-procentig NaOH-15sning en S02- 2— — strom tills pH-vardet har blivit 6,5, orsakar derma lOsnings tillsattning till en lika stor volym vatten, att pH-vardet stiger 'Iran 6,5 till 6,6. Utspades den erhallna losningen anyo med sin egen volym vatten, stiger pH-vitrdet till 6,7 och en tredje upprepning giver pH-var_ det 6,s. Derma relation atergives med ekvationen ln A oH 10 In 9' van A betyder utspadningsfaktorn. I det ovan givna exemplet Oro de successiva utspadningsfaktorerna 2 resp. 4 resp. 8. Ersattes A med 2', 22 och 2', kan man latt faststalla att LlpH = io resp.resp.Den i patentanspraket anforda relationen baseras pa en standardlosning med 8 % NaOH (neutraliseraL). Losningens undre pH-grans är 5,2, vilket redan anforts. Korrekturen for utspadningsmangderna uppgar till: for en 2 °/,;-ig lOsning (A8= 22): InA82111209 = 10 In 2 10 In 2 undre pH-grans = 5,2 + 0,2 = 5,4. for en 32 %-ig limning (A8 --- 2): InA8— 2 In 2 10 ln 210 In 2 undre pH-grans = 5,2— 0,2 =5. In this specification and in the patent claims, the ratio SO 2: NaOH is expressed in pH. This is undoubtedly appropriate and precise, because on the one hand it is quite difficult to determine or define this relationship directly. Small amounts of SO, are carried by the ether during the washing, so that pH feeds are a simple means of regulating the concentration of the wash water. On the other hand, the SO 2 supply involved an acidification, which mediates the decrease of the pH value, so that a given pH corresponds only to a certain ratio of SO 2: NaOH. Consequently, the pH value assumes a correct carpet. For a solution containing 8% NaOH (neutralized), the pH limits are 5.2 and 6.3. If, on the other hand, one works with more diluted or more concentrated solutions than an 8%, a response arises, since a dilution raises the pH value, while the ratio So, NaOH remains constant. In other words, the values for an 8% solution do not stem from a more dilute with the same ratio SO. In such a case, the second value must be stated and likash in any case, where other concentrations are used. Specifying the correct pH values for all solutions simultaneously requires a formula that contains a correction value for the change that occurs upon dilution. This correction value has been determined experimentally. If a 25% NaOH solution is introduced into a SO2-2 stream until the pH value has become 6.5, the addition of this solution to an equal volume of water causes the pH value to rise to 6.5 to 6. 6. If the resulting solution is diluted anyo with its own volume of water, the pH rises to 6.7 and a third repetition gives the pH every 6, s. This relation is returned with the equation ln A oH 10 In 9 'van A means the dilution factor. In the example given above, the successive dilution factors 2 resp. 4 resp. 8. If A is replaced by 2 ', 22 and 2', it can be stated that LlpH = 10 and resp. The ratio in the patent claim is based on a standard solution with 8% NaOH (neutralize L). The lower pH limit of the solution is 5.2, which has already been stated. The correction for the amount of dilution amounts to: for a 2 ° /,; - ig solution (A8 = 22): InA82111209 = 10 In 2 10 In 2 lower pH limit = 5.2 + 0.2 = 5.4. for a 32% gluing (A8 --- 2): InA8— 2 In 2 10 ln 210 In 2 lower pH limit = 5.2— 0.2 = 5.

Standardlosningens koneentration är beraknad sasom NaOH, emedan sammansattning- en av det totala (NaOHS02)-komplexet är obestamd och varierande. Utfores tvattningen med en bisulfitlosning, vans pH endast obetydligt overstiger de givna granserna, avslojar Nesslerprovet omedelbart eterns otillrackliga renhet. The concentration of the standard solution is calculated as NaOH, because the composition of the total (NaOHSO2) complex is undetermined and varies. If the washing is carried out with a bisulfite solution, the pH of which only slightly exceeds the given limits, the Nessler test immediately reveals the insufficient purity of the ether.

Det har visat sig att pa detta satt mycket ren eter kan framstallas. Givetvis ar det mind-re enkelt att halla tvattvatskans pH-varde inom de angivna granserna under hela processen, emedan SO2 kan losas i etern. Det är alltid radligt att genomfora tvattprocessen kontinuerligt och i motstrom. Forfares sã, bringas den praktiskt taget rena etern i kontakt med en farsk losning, som endast i ringa utstrackning fororenas. Darigenom uppnar man, alt atininstone i det sista reningssteget ingen risk fOreligger att pH-vardet gar utanfor de uppgivna granserna. It has been found that in this way very pure ether can be produced. Of course, it is less easy to keep the pH of the wash water within the stated limits throughout the process, since SO2 can be dissolved in the ether. It is always advisable to carry out the washing process continuously and in countercurrent. If so processed, the substantially pure ether is brought into contact with a fresh solution which is only slightly contaminated. In this way, it is achieved that, at least in the last purification step, there is no risk that the pH value goes beyond the stated limits.

For framstallningen av narkoseter är en omedelbar ytterligare tvattning med vatten, torkning och rektifikation av den renade etern nodvandig. Uppskjutes denna behandling nagra dygn, sjunker inangden frainstalld narkoseter betydligt. Det ar alltsa viktigt att tvatta etern med den bisulfit innehallande losningen pft sadant salt, att eterns varaktighet forbattras, sO. att den ieke omedelbart behover vida rebehandlas till narkoseter. Detta kan Astadkornmas genom uppfinningen, forutsatt att den bisulfit innehallande ltisningens pH-varde halles mellan InA(8)InA(8) 5,5 + 10 In 2 och 5,9 + 10 In 2. For the preparation of anesthetic ether, immediate further washing with water, drying and rectification of the purified ether is necessary. If this treatment is postponed for a few days, the incidence of uninstalled anesthetic drops significantly. It is therefore important to wash the ether with the bisulfite-containing solution of such salt that the duration of the ether is improved, so. that it does not immediately need to be re-treated into anesthesia sites. This can be accomplished by the invention, provided that the pH of the bisulfite-containing solution is kept between InA (8) InA (8) 5.5 + 10 In 2 and 5.9 + 10 In 2.

Efter rektifikationen motsvarar 80 % av den erhallna etern kraven pa narkoseter enligt den hollandska farmakopeen, 5. uppl. After rectification, 80% of the ether obtained corresponds to the requirements for anesthesia according to the Dutch Pharmacopoeia, 5th ed.

Exempel. Example.

Sasom utgangsmaterial anvandes en vatska, som innehaller 97 % eter tillsamans med for- oreningar, t. ex. etanol, vatten, aldehyder, omattade foreningar, peroxider saint amnen riled dalig laid. Till tvattningen an-vandes lampligen en natriumbisulfitlosning, framstand genom att losa aasformig svaveldioxid i en 20-procentig natriumhydroxidliisning. Enligt uppfinningen justeras losningens pH till Indian In 8/och 6,310 In In 8 ' 2 5,2 -I- 10 In 2 eller WI Indian 5,2-0,13 och 6,3--0,13. I enlighet med dessa krav avbrytes svaveldioxidgasens inledning, nar losningens pH har sjunkit till 5,4. For att tvatta 1000 liter oren eter enlist inotstrOmsprincipen behoves c:a 450 liter av den framstallda natriumbisulfithaltiga losningen. Den sa renade etern tvattas slutligen med 500 liter vatten och destilleras efter torkning Over kalciumklorid. Darvid uppkommer e :a 900 liter eter, varav 80 % motsvarar renhetskraven enligt den hollandska farmakopeen, 5:e uppl. for eter »ad narcosim» och _resten motsvarar farmakopeens fordringar pa eter till andra andainal. Utan den avslutande tvattningen skulle forhallandet yam 40 % narkoseter och 60 % annan eter. The starting material used was a liquid containing 97% of ether together with impurities, e.g. ethanol, water, aldehydes, unsaturated compounds, peroxides saint amnen riled dalig laid. For the washing, a sodium bisulfite solution was suitably used, obtained by dissolving ash-like sulfur dioxide in a 20% sodium hydroxide solution. According to the invention, the pH of the solution is adjusted to Indian In 8 / and 6.310 In In 8 '2 5.2 -I- In 2 or WI Indian 5.2-0.13 and 6.3--0.13. In accordance with these requirements, the introduction of the sulfur dioxide gas is interrupted when the pH of the solution has dropped to 5.4. In order to wash 1000 liters of crude ether in accordance with the flow principle, approximately 450 liters of the prepared sodium bisulfite-containing solution are needed. The purified ether is finally washed with 500 liters of water and distilled after drying over calcium chloride. This results in about 900 liters of ether, of which 80% corresponds to the purity requirements according to the Dutch Pharmacopoeia, the 5th edition for ether "ad narcosim" and the rest corresponds to the pharmacopoeia's requirements for ether to other spirits. Without the final wash, the ratio would be 40% anesthetic ether and 60% other ether.

Claims (4)

Patentanspra.k:Patentanspra.k: 1. Salt att rena eter, varvid raeter tvattas med en natrium- eller kaliumbisulfit innehallande losning, kannetecknat darav, att pHvardet av den anvanda bisulfit innehallande losningen uppgar till mellan In.A(8)InA(8) 5,2 +och 6,3 + 10 In 210 In 2' varvid A(8) betyder den faktor, soul visar bisulfitlosningens utspadning i jamforelse med en standardlosning med en koncentration av 8 %, beraknad sasom NaOH.Salt to purify ether, the ether being washed with a solution containing sodium or potassium bisulfite, characterized in that the pH of the solution containing bisulfite used is between In.A (8) InA (8) 5.2 + and 6, 3 + 10 In 210 In 2 'where A (8) means the factor, soul shows the dilution of the bisulfite solution in comparison with a standard solution with a concentration of 8%, calculated as NaOH. 2. Satt enligt patentanspraket 1, kannetecknat darav, att tvattningen genomfores kontinuerligt och i motstrom.2. Set according to claim 1, characterized in that the washing is carried out continuously and in countercurrent. 3. Satt att framstalla narkoseter enligt patentanspraken 1 och 2, kannetecknat darav, att den erhallna etern omedelbart tvattas med vatten, torkas och rektifieras. — —33. A method of producing anesthetic ether according to claims 1 and 2, characterized in that the resulting ether is immediately washed with water, dried and rectified. - —3 4. Solt enligt patentanspraken 1 och 2 for framstallning av ren eter med stor -varaktighet, som lampar sig for framstallning av narkoseter medelst tvattning med vatten, torkning och rektifiering, kannetecknat dfirav, att den bisulfit innehallande losningens pH-varde ligger mellan lnA(8)MA(s) -I- 5, 10 ln 2och 5,9 + 10 ln 2' Stockholm 1050. littnal. Bolan P. A. Norsteat S0Act.r 5000004. A salt according to claims 1 and 2 for the production of pure ether of high duration, which is suitable for the preparation of anesthetic ethers by washing with water, drying and rectification, characterized in that the pH value of the bisulfite-containing solution is between 1nA (8 ) MA (s) -I- 5, 10 ln 2och 5,9 + 10 ln 2 'Stockholm 1050. littnal. Bolan P. A. Norsteat S0Act.r 500000
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