SE125527C1

SE125527C1 -

Info

Publication number: SE125527C1
Authority: SE
Publication date: 1949-01-01

Description

Uppfinnare: W. C. Bokhoven. Inventor: W. C. Bokhoven.

Prioritet begard frdn den SO april 1943 (Nederlanderna). Priority was given to SO April 1943 (Netherlands).

FOreliggande uppfinning avser ett Vidaringssatt for rening, t. ex. forbattring av farg, smak och lukt av vatskor, i synnerhet vattenlosningar av organiska amnen, sasom t. ex. bet- oeh rorsoekersafter eller -losningar, 18sningar av glykos, dextros, stdrkelsesocker, maltos, injolksocker och liknande och losningar av organiska syror och deras salter medelst aktivt kol i kornform. The present invention relates to a purification set for purification, e.g. improvement of the color, taste and odor of water lilies, in particular aqueous solutions of organic substances, such as e.g. beet or juice juices or solutions, solutions of glucose, dextrose, starch sugar, maltose, inhaled sugar and the like and solutions of organic acids and their salts by means of activated carbon in granular form.

Vid reningen av sadana valskor med aktivt kol har denna produkt hittills anvants i pulverform. Vid detta anvandningssUt genomfLires behandlingen av vatskan med kolet ofta I motstrOm, varvid sasom bekant reningen mestadels sker i tva eller Hera steg och da fOrst med en redan en eller flera ganger an-valid produkt och darefter med farskt aktivt kol, varigenom en besparing ernas med avseende pa avfargningskostnaderna. I nagra fall genomfOres liven en re,generering av det anvanda pulverkolet, antingen enbart genom kokning eller uppslamning av kolet med Jut och/eller syra eller genom en kombination. dessa kemiska medel med en termisk behandling, namligen en upphettning av materialet till omkring 600° C under uteslutning av tuft. In the purification of such activated carbon roller shoes, this product has hitherto been used in powder form. In this application, the treatment of the liquid with the carbon is often carried out in countercurrent, whereby as is known the purification usually takes place in two or several steps and then first with an already one or more times valid product and then with fresh activated carbon, whereby a saving is made with with respect to the decolorization costs. In some cases, the life is carried out by a re, generation of the used powdered carbon, either only by boiling or slurrying the carbon with Jut and / or acid or by a combination. these chemical agents with a thermal treatment, namely a heating of the material to about 600 ° C with the exclusion of tuft.

Gentemot nackdelarna hos detta i nagon man omstd.ndliga fOrfaringssatt och den tamligen omfangsrika apparaturen i form av omroringskar, filterpressar, efterfilter och eventuellt liven en regenerationsanordning sta emellertid avsevarda fordelar. Den till anvandning kommande kolmangden är namligen ringa och det Or mojligt att genom sma. andringar av denna mangd avsevart utjarana variationerna i kvaliteten hos de for behandling a-vsedda safterna. Dessa senare fordelar gentemot kolonnfiltreringen med benkol i kornform Oro sa betydande, att forfaringssattet med aktivt kol i pulverform under de senaste 25 area bar vunnit mer och mer insteg, fastan kolonnfiltreringen i och for sig uppvisar vissa fortjanster, i synnerhet emedan faire manipulaHoner erfordras under filtreringen och emedan man erhaller filtrat av olika renhetsgra der, vilket ofta Or onskvart vid framstallningen av olika sortiment, sasom är fallet inom sockerraffineringen. Vid anvandningen benkol erfordras emellertid stora mangder (tiotals procent), sa att avfargningsapparaturen maste vara mycket omfangsrik och av ekonomiska skal en regenerering av de utnyttjade kolen arfor maste fOretagas. Uttagandet ur filtren och den termiska regenereringen av dessa stora kolmangder betyder emellertid en avsevard komplikation. Benkolsfiltren och regenerationsugnarna bilda foljaktligen i stora sockerraffinaderier, ddr detta forfaringssalt genomfores, en mycket omfangsrik bidrift. However, in view of the disadvantages of this cumbersome procedure and the rather extensive equipment in the form of agitators, filter presses, after-filters and possibly the life of a regeneration device, there are considerable advantages. The amount of coal that comes into use is small and it is possible to through small. changes in this amount corresponded to the varying variations in the quality of the juices for treatment. These latter advantages over the column filtration with granular bone carbon Oro said significantly that the procedure with activated carbon in powder form during the last 25 years has gained more and more steps, although the column filtration itself shows certain advantages, especially since fair manipulations are required during the filtration. and because filters of different degrees of purity are obtained, which is often the case in the production of different assortments, as is the case in sugar refining. When using bone charcoal, however, large quantities (tens of percent) are required, so that the decolorization equipment must be very extensive and for economic reasons a regeneration of the utilized coal must be carried out. However, the removal from the filters and the thermal regeneration of these large amounts of carbon mean a considerable complication. The charcoal filters and regeneration furnaces consequently form in large sugar refineries, where this process salt is carried out, a very extensive contribution.

Till en anvandning av aktivt kol i kornform for rening av valskor, vartill foreliggande ansokning hOnfOr sig, har man i praktiken ieke kommit och detta av den orsaken, att i brist pO. en god regenereringsmetod detta forfarande med aktivt kol I kornform skulle yarn oekonomiskt pa grund av den storre mangd, som ddrvid anvandes, och kornkolets bogre pris i jamforelse med anvandningen av aktivt kol i pulverform. Den vid benkol anvanda regenerationen i glikluguar medf Or pa grund av den mjukare beskaffenheten hos det vegetabiliska, aktiva kolets korn mycket storre svarigheter an regenerationen av benkolet. Den enda praktiska anvandningen av det aktiva kolet i kornform i ovannamnda avseende är den vid reningen av vatten i andamal att avlagsna smak- och luktamnen, spar av olja eller overskott av klor, varvid det icke är fraga om a-vlagsnandet av fargamnen, och i mindre skala aven for forbattring av fargen. I det senare fallet sker emellertid ingen regenerering. In practice, there has been no use of activated carbon in granular form for the purification of roller shoes, to which the present application is based, and this for the reason that in the absence of pO. a good regeneration method this process with activated carbon in granular form would be economical due to the larger amount used therewith and the higher price of granular carbon compared to the use of activated carbon in powder form. Due to the softer nature of the grains of activated carbon, bone regeneration used in bone charcoal has much greater similarities than the regeneration of bone char. The only practical use of the activated carbon in granular form in the above-mentioned respect is that in the purification of water in andamal to remove the flavors and odors, save oil or excess chlorine, in which case there is no question of the a-removal of the dyes, and in smaller scale aven for color improvement. In the latter case, however, no regeneration takes place.

Man har nu funnit, att det aven med avseende pa de i inledningen namnda vatskorna Or mojligt, att framgangsrikt anvanda kolonnfiltreringen for aktivt kol i kornform, om man anvander ett aktivt kol i form av korn med en storlek av 1--3 mm med vissa egenskaper, vilket tillater att vid regenerationen — — av den utnyttjade produkten undvika en termisk behandling i sarskilda ugnar. Darvid kunna filterna vid samma avfargningskapacitet pa grund av kolets storre avfargningsformaga vara mycket mindre, an vid anyandningen av benkol. Forfaringssattet enligt uppfinningen bestar dari, att man leder den for rening avsedda vatskan, i synnerhet en. vattenlosning av ett organiskt amne, sasom betoch rorsockersafter, resp. -losningar, losningar, av andra sockerarter och losningar av organiska syror eller deras salter, genom en eller flera kolonner, vilka aro fyllda med ett aktivt kol i kornform, vilket i torrt tillstand har en litervikt av hogst 250 g, har ett vatningsvarme for bensol av minst 23 kalorier per g torrt kol, uppvisar en bensoladsorption vid 20° C ur en vid denna temperatur till 92,7 % med bensol mattad luftstrom av minst 60 g per 100 g torrt kol, och regenererar fullstandigt eller delvis utnyttjade kol in situ genom en behandling med en alkalisk vatska, eventuellt under efterbehandling med syra. I allmanhet är en kornstorlek av 0,s-1,5 ram lamplig. Genom anvandningen av ett aktivt kol av den angivna strukturen ernas 8verraskande nog enligt foreliggande forfaringssatt i forsta hand, att en viss avfargningsverkan ernas med en kolmangd, lika stor eller mindre an den, vii-ken erfordras av det vanliga, pulverformiga avfargningskolet, under det att det vidare her visat sig, att detta kornkol kan regenereras pa rent kemisk vag, utan att kolet behover uttagas ur filtren. It has now been found that it is also possible, with respect to the water shoes mentioned in the introduction, to successfully use the column filtration for activated carbon in granular form, if one uses an activated carbon in the form of granules with a size of 1-3 mm with certain properties, which allows to avoid thermal treatment in special furnaces during the regeneration - - of the product used. In this case, the filters at the same decolorizing capacity due to the larger decolorizing capacity of the carbon can be much smaller, than with the use of bone charcoal. The method according to the invention consists in guiding the liquid intended for purification, in particular one. dehydration of an organic substance, such as beet sugar juice, resp. solutions, solutions, of other sugars and solutions of organic acids or their salts, through one or more columns, which are filled with an activated carbon in granular form, which in the dry state has a liter weight of at most 250 g, has a heating water for benzene of at least 23 calories per g of dry carbon, exhibits a benzene adsorption at 20 ° C from a at this temperature to 92.7% gasoline-laden air stream of at least 60 g per 100 g of dry carbon, and regenerates fully or partially utilized carbon in situ by a treatment with an alkaline liquid, possibly during post-treatment with acid. In general, a grain size of 0, s-1.5 frame is suitable. By the use of an activated carbon of the indicated structure, surprisingly according to the present method, in the first place, a certain decolorizing effect with an amount of carbon, equal to or less than that required by the usual, powdered decolorizing carbon, while it has further been shown here that this grain carbon can be regenerated in a purely chemical way, without the carbon having to be removed from the filters.

Det for foreliggande forfaringssatt for anvandning avsedda, aktiva kolet i kornform skall jamte en stor inre yta, vilken bestammer avfargningsformagan, aga ett stort antal porer av mindre eller storre dimensioner, vilka senare tjana som forbindelsevagar till den inre ytan. Genom narvaron av detta stora antal forbindelseporer, vilkas dimensioner icke skola vara for sma, kunna aven de i den for rening avsedda vatskan i form av molekylkomplex foreliggande fororeningarna uppna hela den inre kolytan. I olika soaker- och glykoshaltiga vatskor foreligger fargamnet ofta I denna form och man ernar da enligt foreliggande forfaringssatt en lika god avfargningsverkan som med starkt aktivt pulverkol, vars inre yta pa grund av partiklarnas sma dimensioner i och for sig dr snabbare och lattare tillganglig fOr de namnda fororeningarna. En vidare for praktiken mycket viktig verkan hos denna speciella struktur be-star dari, att de vid kolets yta adsorberade fororeningarna battre kunna avlagsnas genom de for anvandning avsedda regenereringsvatskorna an yid kornformigt, aktivt kol med en tatare struktur. The activated carbon for use in the present process, together with a large inner surface, which determines the decolorizing shape, will form a large number of pores of smaller or larger dimensions, which later serve as connecting scales to the inner surface. Due to the presence of this large number of connecting pores, the dimensions of which should not be too small, the impurities present in the liquid intended for purification in the form of molecular complexes can also reach the entire inner carbon surface. In various soaker- and glucose-containing liquids the dye is often present in this form and the present process gives as good a decolorizing effect as with strongly activated powdered carbon, the inner surface of which due to the small dimensions of the particles itself is faster and easier to access. named pollutants. A further very important effect for practice of this special structure is that the contaminants adsorbed on the surface of the coal can be better removed by the regeneration liquids intended for use from granular, activated carbon with a tartar structure.

Det har visat sig, att denna regenerering, vilken kan genomforas med lut vid hogre ternperatur och eventuellt kombineras med en efter- eller forbehandling med syra, vid det enligt foreliggande uppfinning anvanda aktiva kolet i kornform forloper sâ latt och med sh gott resultat, att den kan forsigga in situ, och att man kan aysta fran en termisk regenerering. Det har vid undersokningarna pa detta omrade vidare visat sig, att narvaron av lyofila kolloider och i allmanhet av amnen, vilken i den for behandling avsedda vatskan framkalla en stark »Tyndalleffekb, skola undvikas. Sasom sadana aro sarskilt aggviteamnen, respektive aggviteartade amnen, pektin o. s. v. att betrakta. Det har fastslagits, att dessa fororeningar, vilkas partiklar aro avsevart storre an de hos det for avlagsnande avsedda fargamnet, stoppa till fOrbindelseporerna pa sadant satt och aro sa svara att avlagsna, att en langtgaende regenerering med lut in situ under vissa omstandigheter Or mycket svâr aven for det ifragavarande kolet. Det Or dad& under vissa forhallanden erforderligt att forbehandla vatskan med hydrofila adsorberande amnen, sasom t. ex. bentonit, blekjord o. s. v., vilka eventuellt f8rut have undergatt en behandling respektive rening. Dessutom kunna dessa grovdispersa, kolloidala fororeningar i langden Oka filtermotstandet icke ovasentligt. Genom de ovannamnda iakttagelserna kan det forklaras, att yid anyandningen av ett tatare eller finare porOst kornkol med samma kornstorlek den inre ytan in eller blir for litet tillganglig, och att avfargningsverkan darigenom minskas f Or hastigt. Dessutom kunna I detta fall de yid kolets yta adsorberade fororeningarna med storre svarighet resp. mycket mindre fullstandigt avlagsnas med lut och syra. It has been found that this regeneration, which can be carried out with lye at a higher temperature and possibly combined with a post- or pre-treatment with acid, in the activated carbon used in granular form according to the present invention proceeds so slowly and with good results that it can proceed in situ, and that one can aysta from a thermal regeneration. It has further been shown in the investigations in this field that the presence of lyophilic colloids and in general of the substances which in the liquid intended for treatment produce a strong "Tyndalle effect" should be avoided. As such, the aggvate substances, aggregate substances, pectin, etc., in particular, are to be considered. It has been found that these contaminants, the particles of which are considerably larger than those of the dye intended for removal, stop at the connection pores in such a way and are so responsible for the removal that a far-reaching regeneration with lye in situ under certain circumstances is very difficult. for the coal in question. Under certain conditions it is necessary to pre-treat the liquid with hydrophilic adsorbent substances, such as e.g. bentonite, bleached earth, etc., which may have previously undergone a treatment or purification, respectively. In addition, these coarsely dispersed, colloidal contaminants in the long run increase the filter resistance not insignificantly. From the above-mentioned observations it can be explained that the use of a tatter or finer porosity grain coal with the same grain size enters the inner surface or becomes too little accessible, and that the decolorizing effect is thereby reduced too rapidly. In addition, in this case the contaminants adsorbed by the surface of the yid carbon with greater similarity resp. much less completely removed with lye and acid.

For genomfOrandet av fOreliggande Odaringssatt ledes den for avf arguing avsedda vatskan sedan den, om sa erfordras, har blivit forrenad med bentonit eller liknande, genom en eller flera kolonner med det aktiva kornkolet, tills kolets adsorptionsformaga till starsta delen blivit uttomd. For regenerering av kolet ledes, efter foretradesvis sa fullstandig uttvattning som mojligt av den kvarblivande vatskan, utspadd lut vid forh8jd temperatur langsamt genom massan. Eventuellt kan i anslutning hirtill efter uttvattning cv luten med vatten en behandling med utspadd syra foretagas, varefter man likaledes eftertvattar med vatten. Vid alla dessa behandlingar är det alltsa onodigt att taga ut kolet ur apparaten. Det har visat sig, att adsorptionsformagan hos det enligt uppfinningen anvanda kolet av speciell struktur pO. detta salt I manga fall kan aterstallas praktiskt taget fullkomlig, sa att kretsloppet avfargningsregenerering kan upprepas flera ganger. I vissa fall kan vid den forsta behandlingen en ringa minskning av adsorptionsformagan figa rum. Vid de fortsatta behandlingarna minskas emellertid joke adsorptionsfOrmagan ytterligare. — —3 Det for anvandning avsedda kolet skall lampligen hava en kornstorlek av icke Over 2 mm. Med avseende pa de ovan namnda betingelser, som skola uppfyllas av kolet, skall ytterligare foljande framhallas. For carrying out the present Odaringssatt, the liquid intended for disposal is passed after it, if required, has been contaminated with bentonite or the like, through one or more columns with the activated carbon, until the adsorption capacity of the carbon has largely been exhausted. For regeneration of the coal, after preferably as complete a dewatering as possible of the remaining liquid, diluted lye at elevated temperature is passed slowly through the mass. Possibly, in connection with this, after dilution or lye with water, a treatment with dilute acid can be carried out, after which it is also re-washed with water. In all these treatments, it is therefore unnecessary to remove the carbon from the appliance. It has been found that the adsorption formag of the carbon of special structure pO used according to the invention. this salt In many cases can be recovered practically completely, so that the cycle of decolorization regeneration can be repeated several times. In some cases, on the first treatment, a slight reduction in the adsorption capacity may occur. With the continued treatments, however, the joke adsorption capacity is further reduced. - —3 The coal intended for use shall suitably have a grain size not exceeding 2 mm. With regard to the above-mentioned conditions, which must be met by coal, the following should be further emphasized.

Litervikten, d. v. s. antalet g torrt kol per liter skall bestammas, sedan kolkornen hopskakats till en konstant volym. The liter weight, i.e. the number of g of dry coal per liter, must be determined after the coal grains have been shaken to a constant volume.

Vatningsvarmet for bensol bestammes pa sfi. Ott, att man inf5r kornkolet, vars porer aro fyllda med hilt, i flytande bensol. Det ar namligen kant, att man vid aktivt kol finner ett hogre vatningsvarme, om man i forvag evakuerar kolet. The irrigation heat for benzene is determined on sfi. Note that the charcoal, the pores of which are filled with hilt, is introduced into liquid benzene. Namely, it is an edge that with activated carbon you find a higher heat of irrigation, if you evacuate the carbon in advance.

Bensoladsorptionen vid 20° C i en till 92,7med bensol mattad luftstrOm bestam- mes darigenom, att man leder en blandning av torr luft och bensolanga, vilken innehaller 297 g bensol per m' vid 0 sh. hinge Over 100 g torrt kol, tills vikten has detta icke mera Ran Nar kolet motsvarar den fordran, att denna bensoladsorption uppgar till minst 60 g per 100 g torrt kol, ar de verksamma porernas volym upp till ett tvarsnitt av 50 milli- mikron minst 68 cm' per 100 g kol. Om dess- utom volymen av alla porerna, alltsa inklusive de, vilka aro st5rre an 50 millikron, uppgar till 200 cm' eller mer per 100 g torrt kol, fir kolet sarskilt lampligt for foreliggande fOrfaringssatt. The benzene adsorption at 20 ° C in a stream of air fed to 92.7 with benzene is determined by passing a mixture of dry air and benzene long, which contains 297 g of benzene per m 'at 0 sh. When the carbon corresponds to the requirement that this benzene adsorption amounts to at least 60 g per 100 g of dry carbon, the volume of the active pores up to a cross-section of 50 millimicrons is at least 68 cm 'per 100 g of col. In addition, if the volume of all the pores, including those larger than 50 millicrons, amounts to 200 cm 3 or more per 100 g of dry carbon, the carbon is particularly suitable for the present process.

I synnerhet for glykos- och sackraroslosningar ãr det lampligt att forrena vatskan fore filtreringen, emedan densamma innehal- ler grovdispersa, kolloidala fororeningar. Emedan man enligt foreliggande forfarings- satt regenererar uteslutande kemiskt, sker ingen forstoring av de kvarblivande fororeningarna genom glodgning. Vidare kan det re- kommenderas att i fOrvag avlagsna metallf8r- eningar, sasom t. ex. jarnkomplexer. Sasom fOrreningsmedel kan man f8rutom de redan namnda hydrofila, adsorberande amnena aven anvanda aktivt kol i pulverform, foretradesvis med ett stort antal parer med storre di- mensioner, och andra kolhaltiga filtrerings- medel, sasorn t. ex. vid lag temperatur med kemikalier behandlade kolhaltiga material, mineraliska reningsmedel, sasom t. ex. preci- pitater av kalciumfosfat, kalciumsulfit, kalciumkarbonat och aluminiumdioxid, foretra.- desvis i gelform, eller kombinationer av tva eller flera av dessa amnen. I sarskilda fall kan man foretaga en efterbehandling ay de enligt uppfinningen erhallna filtraten med av- fdrgningskol, vilken efterbehandling kan genomf5ras saval i suspension som i efterfilter. FOr att Oka kornkolets genomsnittsbelastning kan man, sasom ar vanligt yid benkolfil- treringen, koppla tva eller flera filter efter vat- andra. Nar det fOrkopplade filtret är praktiskt taget utnyttjat, urtvattas det med vatten och regenereras i anslutning dartill. Det andra filtret anvandes dâ sasom Milner framfor ett med filter med nyregenererat kol. Enligt en ytterligare utforingsform av uppfinningen kan man belasta kolet endast sa langt, att detta i genomsnitt endast ar delvis utnyttjat. Om det t. ex. ar mojligt, att liana ett filter i drift ett visst antal dagar, innan detsamma ar fullstandigt utnyttjat, salter man i detta fall filtret ur drift, sedan det t. ex. har varit i drift en tredjedel av namnda tid. Filtreringen av de for behandling avsedda Vatskorna genom kolonnen kan ske saval nedifran och uppat som uppifran och nedat. I allmanhet fir det lampligt, att icke taga kontakttiden, vii-ken for ovrigt ar beroende av slaget av de f Or behandling avsedda vatskorna (i synnerhet av viskositeten) och den anvanda temperaturen, for kort. I de fiesta fall ãr en skenbar kontakttid av en halv timme eller langre onskvart, vilket innebar, att icke mer an 2 m' av den for behandling avsedda vatskan skall filtreras per timme genom ett filter enligt uppfinningen per m' av filterinnehallet. Particularly for glucose and sucrose solutions, it is appropriate to purify the liquid before filtration, since it contains coarsely dispersed, colloidal impurities. Since, according to the present procedure, it is regenerated exclusively chemically, no enlargement of the remaining contaminants takes place by annealing. Furthermore, it can be recommended that metal compounds be removed in advance, such as e.g. iron complexes. In addition to the already mentioned hydrophilic, adsorbent substances, activated carbon in powder form can also be used as the purifying agent, preferably with a large number of pairs with larger dimensions, and other carbonaceous filtering agents, e.g. at low temperatures with chemicals treated carbonaceous materials, mineral cleaners, such as e.g. precipitates of calcium phosphate, calcium sulphite, calcium carbonate and alumina, preferably in gel form, or combinations of two or more of these substances. In special cases, a post-treatment can be carried out on the filtrates obtained with the charcoal obtained according to the invention, which after-treatment can be carried out both in suspension and in after-filter. In order to increase the average load of the coal, it is possible, as is usual in bone charcoal filtration, to connect two or more filters one after the other. When the connected filter is practically used, it is diluted with water and regenerated in connection therewith. The second filter was then used as Milner instead of one with a filter with newly regenerated carbon. According to a further embodiment of the invention, the carbon can be loaded only to such an extent that this is on average only partially utilized. If it e.g. It is possible to leave a filter in operation for a certain number of days before it is fully utilized, in this case the filter is salted out of operation, since it e.g. has been in operation one third of the said time. The filtration of the Vatskorna intended for treatment through the column can take place from below and upwards as well as from above and downwards. In general, it is appropriate not to take the contact time, which otherwise depends on the type of water shoes intended for treatment (in particular on the viscosity) and the temperature used, too short. In most cases, an apparent contact time of half an hour or longer is a quarter of an hour, which means that no more than 2 m 'of the liquid to be treated is to be filtered per hour through a filter according to the invention per m' of the filter contents.

Regenereringen foretages foretradesvis med varm lut. Alltefter den av kornkolet avfargade vatskans slag, av vilken i praktiken alltid spar kvarbliva i kolet, och efter det adsorberande amnets art valjer man temperaturen vid lutregenereringen I. ex. till mellan 50 och 9° C. I vissa fall an det lampligt att anvanda ternperaturer Over 100° C, varvid regenereringen sker under tryck. Regenereringsvatskorna ledas genom kolonnen foretradesvis i motstrom mot den for rening avsedda vatskan. Koncentrationen hos den lutlosning, som skall anvandas for regenereringen, kan t. ex. uppga till omkring 0,05 till 5 % och den for syralOsningen till omkring 0,05 till 3 %. For regenereringen av kornkolet, vilket har anvants for rening av glykostunnsaft, anvandes t. ex. foretradesvis icke flagon hogre luftkoncentration an som motsvarar 0,5 NaOH yid en temperatur av ungefar 65° C. Den alkaliska losningen kan eventuellt amen innehalla oxidationsmedel, t. ex. superoxid. Vid regenereringen tvattar man mestadels 3 ganger med vatten, forsta gangen for att grundligt avlagsna aterstoderna av den i kolet befintliga vatskan, den andra gangen for att urspola luten sa mycket som mojligt oak den tredje &igen, for att avlagsna den annu forefintliga syran. I nagra fall ar en svagt sur reaktion hos kornkolet i filtren onskvard och den sista tvattningen kan begransas. Om kolet, t. ex. for behandling ay raffinadlosningar, efter regenereringen ger skall vara fullkomligt neutralt, kan man eftertvatta med en buffertiosning med det erf orderliga pH-vardet. Eventuellt kan lutbehandlingen aven dessutom foregas av en syrabehandling. Uppfinningen skall f8rklaras i anslutning till ett exempel. The regeneration is preferably carried out with hot lye. Depending on the type of water discolored by the charcoal, of which in practice spades always remain in the carbon, and according to the nature of the adsorbent substance, the temperature of the lye regeneration is chosen. to between 50 and 9 ° C. In some cases it is advisable to use temperatures above 100 ° C, whereby the regeneration takes place under pressure. The regeneration liquids are passed through the column preferably in countercurrent to the purification liquid. The concentration of the lye solution to be used for the regeneration can e.g. to about 0.05 to 5% and that for the acid solution to about 0.05 to 3%. For the regeneration of the coal, which has been used for the purification of glycosine barrel juice, e.g. preferably not a higher air concentration corresponding to 0.5 NaOH at a temperature of about 65 ° C. The alkaline solution may optionally contain oxidizing agents, e.g. superoxide. During the regeneration, it is usually washed 3 times with water, the first time to thoroughly remove the residues from the liquid present in the carbon, the second time to rinse out the lye as much as possible, and the third & again, to remove the still existing acid. In some cases, a slightly acidic reaction of the coal in the filters is desirable and the last washing can be limited. About the coal, e.g. for treatment ay refining solutions, after the regeneration gives the shell to be completely neutral, it can be washed with a buffer thawing with the required pH value. The lye treatment may also be carried out by an acid treatment. The invention will be explained in connection with an example.

Exemp el . Example el.

Den fran konvertern kommande glykostunnsaften av omkring ° Bx forsattes med omkring 0,5 % bentonit, raknat pa torrsub- — l25527 — stans. Saften neutraliseras till ett pH-varde av 5,7 och filtreras genom ett vanligt filter. Den forrenade tunnsaften, vilken t. ex. har en. farg av 1,s° Stammer per 100 g torrsubstans i 100 cm', installes pa ett prd-varde av 4,2 och ledes med en filtreringshastighet av 1 liter per timme nedifran och uppat genom 1 liter aktivt kol med de ovannananda egenskaperna yid en skikthOjd av 50 cm. Temperaturen vid perkolationen uppgar till 50° C. Filtreringen fort-sates tills filtratets farg är 0,1° Stammer. Filtratmdngden uppgar dd. till 33 liter med en genomsnittsfarg av 0,04° Stammer. For att re0-enerera kolet ledes forst vatten med en temperatur av 55° C uppifrdn och neda't genom kolet, tills filtratet praktiskt taget icke mer uppvisar nagon reaktion med Fehlingslosning. Darefter perkoleras sh Hinge i samma riktning med en. 0,4 %-ig natronlut yid 50° C, att praktiskt taget icke mer flagon farg avgives av kolet. Kolet tvattas med vatten, tills filtratet uppvisar en endast svagt alkalisk reaktion, perkoleras med 0,4 %-ig saltsyra vid c:a 50° C, tills filtratets pH-varde uppgar till onakring 4 och tvdttas Ater med varmt vatten for avlagsnande av saltsyran.. Det har visat sig, att kolet, sedan det blivit belastat och regenererat 30 ganger, fortfarande har formaga, att avgiva samma mangd filtrat med en genomsnittsfarg under 04° Stammer, och alltsa icke uppvisar flagon nomnvard nedsittning av adsorptionsfOrmagan, vara-v framgar, att regenereringen alltid är mycket fullstandig. The glycol barrel juice of about 0 Bx coming from the converter was continued with about 0.5% bentonite, shaved on dry substance. The juice is neutralized to a pH of 5.7 and filtered through a standard filter. The purified barrel juice, which e.g. has a. color of 1, s ° Strains per 100 g of dry matter in 100 cm ', installed at a pr-value of 4.2 and passed at a filtration rate of 1 liter per hour from below and up through 1 liter of activated carbon with the above properties yid a layer height of 50 cm. The temperature at the percolation is 50 ° C. Filtration is continued until the color of the filtrate is 0.1 °. The filtrate quantity states dd. to 33 liters with an average color of 0.04 ° Strains. In order to re-generate the carbon, water with a temperature of 55 ° C is first passed up and down through the carbon, until the filtrate practically no longer shows any reaction with Fehlingslosning. Then sh Hinge is percolated in the same direction with a. 0.4% sodium hydroxide solution at 50 ° C, that practically no more flaky color is given off by the carbon. The carbon is washed with water until the filtrate shows only a slight alkaline reaction, percolated with 0.4% hydrochloric acid at about 50 ° C, until the pH of the filtrate rises to about 4 and washed again with hot water to remove the hydrochloric acid. .. It has been found that the carbon, after being charged and regenerated 30 times, has still been able to give off the same amount of filtrate with an average color below 04 ° Strains, and thus does not exhibit a nominal decrease in adsorption capacity, , that the regeneration is always very complete.

De pa detta satt erhallna safterna giva efter indunstning i vakuum anda till omkring 80 85° Bx an blank sirap med sarskilt ren smak. The juices obtained in this way give after evaporation in a vacuum spirit to about 80 85 ° Bx a shiny syrup with a particularly pure taste.

Vid behandlingen av socker-raffinadlosningar slier a-vfargningen foretradesvis vid 80-85° C och regenereringen vid en sa hijg temperatur som mojligt, t. ex. yid 9° C. Vid behandlingen av andra losningar anpassas behandlingstemperaturen till dessa losningars egenskaper. In the treatment of sugar-refined solutions, the α-decolorization preferably slides at 80-85 ° C and the regeneration at as high a temperature as possible, e.g. yid 9 ° C. When treating other solutions, the treatment temperature is adapted to the properties of these solutions.

Claims

Patent claim:

1. added during decolorization and further purification of water-shoes, in particular aqueous solutions of organic substances, such as sugars, organic acids and their salts, can ddray, that one. leads the liquid through one or more columns, which are filled with activated carbon in granular form, the villi in the dry state has a liter weight of at most 250 g, an irrigation value for benzene of at least 23 calories per g of dry carbon and a benzene adsorption of 20 ° C in a at this temperature to 92.7% with benzene-matted air stream of at least 60 g per 100 g of dry carbon, and regenerates the completely or partially dehydrated carbon in situ by treatment with an alkaline liquid.

2. According to patent claim 1, there is a sign that the roller is freed from colloidal contaminants as much as possible in advance.

3. According to patent claims 1-2, it can be concluded that the apparent contact time between liquid and carbon during purification amounts to at least half an hour.

4. set according to patent claims 1-2, characterized in that after the treatment of the fully or partially utilized carbon with an alkaline liquid, a post-treatment with oxygen is carried out.

5. According to patent claims 1-4, Winneteeknat claimed that in the treatment of glucose salts the utilized and with water as completely as possible diluted the coal was treated at a temperature below 60 G with sodium hydroxide solution, the concentration of which does not exceed 1%. Stockholm 1949. Kungl. Boktr. P. A. Norstedt & Soner 490089