CS211141B1 - Method of removal of sulphur dioxyde,copper and colloidal turbid substances out from wine,fruit and other destillates - Google Patents
Method of removal of sulphur dioxyde,copper and colloidal turbid substances out from wine,fruit and other destillates Download PDFInfo
- Publication number
- CS211141B1 CS211141B1 CS272880A CS272880A CS211141B1 CS 211141 B1 CS211141 B1 CS 211141B1 CS 272880 A CS272880 A CS 272880A CS 272880 A CS272880 A CS 272880A CS 211141 B1 CS211141 B1 CS 211141B1
- Authority
- CS
- Czechoslovakia
- Prior art keywords
- distillate
- calcium
- wine
- fruit
- copper
- Prior art date
Links
- 238000000034 method Methods 0.000 title claims description 14
- 235000014101 wine Nutrition 0.000 title claims description 6
- 235000013399 edible fruits Nutrition 0.000 title claims description 4
- 239000010949 copper Substances 0.000 title description 7
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title description 4
- 229910052802 copper Inorganic materials 0.000 title description 4
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 title 1
- 239000005864 Sulphur Substances 0.000 title 1
- 239000008130 destillate Substances 0.000 title 1
- 239000000126 substance Substances 0.000 title 1
- 239000011575 calcium Substances 0.000 claims description 25
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 claims description 24
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 15
- 229910052791 calcium Inorganic materials 0.000 claims description 14
- 239000000725 suspension Substances 0.000 claims description 8
- 239000002253 acid Substances 0.000 claims description 7
- 238000004821 distillation Methods 0.000 claims description 7
- 150000007513 acids Chemical class 0.000 claims description 4
- 239000000292 calcium oxide Substances 0.000 claims description 4
- 235000015096 spirit Nutrition 0.000 claims description 4
- 239000000920 calcium hydroxide Substances 0.000 claims description 3
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims description 3
- 239000000047 product Substances 0.000 claims description 3
- 239000000706 filtrate Substances 0.000 claims description 2
- 238000001914 filtration Methods 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 230000001376 precipitating effect Effects 0.000 claims description 2
- ODINCKMPIJJUCX-UHFFFAOYSA-N Calcium oxide Chemical compound [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims 6
- 235000012255 calcium oxide Nutrition 0.000 claims 3
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 description 8
- 235000002906 tartaric acid Nutrition 0.000 description 8
- 239000011975 tartaric acid Substances 0.000 description 8
- 239000002244 precipitate Substances 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 4
- 238000000855 fermentation Methods 0.000 description 4
- 230000004151 fermentation Effects 0.000 description 4
- 239000000758 substrate Substances 0.000 description 3
- IKHGUXGNUITLKF-UHFFFAOYSA-N Acetaldehyde Chemical compound CC=O IKHGUXGNUITLKF-UHFFFAOYSA-N 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 2
- 159000000007 calcium salts Chemical class 0.000 description 2
- GUPPESBEIQALOS-UHFFFAOYSA-L calcium tartrate Chemical compound [Ca+2].[O-]C(=O)C(O)C(O)C([O-])=O GUPPESBEIQALOS-UHFFFAOYSA-L 0.000 description 2
- 235000011035 calcium tartrate Nutrition 0.000 description 2
- 239000001427 calcium tartrate Substances 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- LELOWRISYMNNSU-UHFFFAOYSA-N hydrogen cyanide Chemical compound N#C LELOWRISYMNNSU-UHFFFAOYSA-N 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000010979 pH adjustment Methods 0.000 description 2
- KJFMBFZCATUALV-UHFFFAOYSA-N phenolphthalein Chemical compound C1=CC(O)=CC=C1C1(C=2C=CC(O)=CC=2)C2=CC=CC=C2C(=O)O1 KJFMBFZCATUALV-UHFFFAOYSA-N 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 108010010803 Gelatin Proteins 0.000 description 1
- 229920000877 Melamine resin Polymers 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 229910001854 alkali hydroxide Inorganic materials 0.000 description 1
- 150000008044 alkali metal hydroxides Chemical class 0.000 description 1
- 239000000440 bentonite Substances 0.000 description 1
- 229910000278 bentonite Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 239000008273 gelatin Substances 0.000 description 1
- 229920000159 gelatin Polymers 0.000 description 1
- 235000019322 gelatine Nutrition 0.000 description 1
- 235000011852 gelatine desserts Nutrition 0.000 description 1
- 239000000017 hydrogel Substances 0.000 description 1
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 150000002978 peroxides Chemical class 0.000 description 1
- 239000000276 potassium ferrocyanide Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 239000010802 sludge Substances 0.000 description 1
- LSNNMFCWUKXFEE-UHFFFAOYSA-L sulfite Chemical class [O-]S([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-L 0.000 description 1
- XOGGUFAVLNCTRS-UHFFFAOYSA-N tetrapotassium;iron(2+);hexacyanide Chemical compound [K+].[K+].[K+].[K+].[Fe+2].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-] XOGGUFAVLNCTRS-UHFFFAOYSA-N 0.000 description 1
- 238000004448 titration Methods 0.000 description 1
Landscapes
- Removal Of Specific Substances (AREA)
- Distillation Of Fermentation Liquor, Processing Of Alcohols, Vinegar And Beer (AREA)
Description
Predmetom vynálezu je nový spfisob odstraňovania kysličníka siřičitého a médi z vinných, ovocných a iných destilátov pomoeou hydroxidu vápenatého alebo CaO, s následovnou úpravou pH a vyzrážaním přebytku vápnika pomoeou kyselin.SUMMARY OF THE INVENTION The present invention provides a novel method of removing sulfur dioxide and media from wine, fruit and other spirits by means of calcium hydroxide or CaO, followed by pH adjustment and precipitation of excess calcium by acid.
Kvasné substráty rfizneho druhu, ako aj vína určené na destiláeiu konzervujú sa kysličníkom siřičitým, čo sa v priebehu uskladnenia viackrát opakuje, v dfisledku čoho mávajú vysoký obsah SOg. Kysličník siřičitý je prchavý a při destilácii prechádza do destilátu, čo sa velmi nepríjemne prejavuje vo vfini a chuti destilátu. Okrem toho je kysličník siřičitý velmi agresívny a koroduje destilačné zariadenia, čím sa tieto rýchle opotřebovávájú a okrem toho uvolňuje sa do destilátu nežiadúce množstvo médi. Destiláty so zvýšeným obsahom médi sú menej kvalitně a velmi tažko sa predávajú najma na zahraničnom trhu.Fermented fermentation substrates as well as wines intended for distillation are conserved with sulfur dioxide, which is repeated several times during storage, as a result of which they have a high SOg content. Sulfur dioxide is volatile and passes into the distillate during distillation, which is very unpleasant in the taste and taste of the distillate. In addition, the sulfur dioxide is very aggressive and corrodes the distillation apparatus, whereby these wear out rapidly and, moreover, undesirable amounts of medium are released into the distillate. Spirits with increased media content are of lower quality and very difficult to sell especially on the foreign market.
Doteraz známe postupy neodstránia dostatočne kysličník siřičitý a meá z vinných a ostatnýeh destilátov a okrem toho nepriaznlvo ovplyvňujú kvalitu destilátov. Napr. odstraňovanie SOg pomoeou peroxidu vodíka (HgOg) spfisobuje zhoršenie kvality destilátu a okrem toho peroxid mfiže oxidovat etylalkohol na acetaldehyd.The prior art processes do not sufficiently remove sulfur dioxide and from wine and other spirits and, in addition, adversely affect the quality of the spirits. E.g. removal of SOg with hydrogen peroxide (HgOg) causes a deterioration in the quality of the distillate and, moreover, the peroxide can oxidize ethyl alcohol to acetaldehyde.
Ďalším nedostatkom doterajších spfisobov je, že destiláty obsahujú zvýšený obsah médi. Doteraz známým postupom pomoeou ferokyanidu draselného je možné čiastočne odstrénit z destilátu meá. Odstránenie médi nie je vždy dostatočne účinné a okrem toho, takto ošetřené destiláty mfižu obsahovat kyanovodík, ktorý je prchavý a aj pri opakovanej rektifikécii prechádza do destilátu.A further drawback of the prior art is that distillates contain an increased medium content. The prior art potassium ferrocyanide method can partially remove the copper distillate. Removal of the medium is not always sufficiently effective and, moreover, the distillates treated in this way may contain hydrogen cyanide which is volatile and passes into the distillate even after repeated rectification.
Nevýhody doterajších postupov pri výrobě destilátov odstraňuje spfisob podl’a vynálezu, ktorý spočívá v tom, že do destilátu sa přidá hydroxid vápenatý Ca(0H)2, zamieša a nechá reagovat, pričom sa vyzráža kysličník siřičitý a meá. PodTa potřeby mflže sa tento postup doplnit čeriaoimi prostriedkami napr. 0,25 g.l-' hydrogelu bentonitu a ,0 mg.l-' želatiny, čím sa urýchli sedimentáeia kalov. Upravený destilát sa přefiltruje a> přidá sa do něho kyselina, účinkom ktorej sa vyzrážajú přebytky vápnika vo formě vápenatých soli a upraví sa pH na požadovaná mieru. Úprava pH je možná aj v- kombinácii s C02 a kyselinou vinnou, připadne inými kyselinami.The disadvantages of the prior art distillate production processes are eliminated by the method according to the invention which comprises adding Ca (OH) 2 calcium hydroxide to the distillate, mixing and reacting, precipitating sulfur dioxide and having a precipitate. If desired, this process may be supplemented with blackening agents, e.g. 0.25 g - bentonite hydrogel and 0 mg.l - gelatin to accelerate sludge sedimentation. The treated distillate is filtered and acid is added to precipitate excess calcium in the form of calcium salts and adjust the pH to the desired level. PH adjustment is also possible in combination with CO 2 and tartaric acid or other acids.
Použitím spdsobu podTa vynálezu odstráni sa z destilátu kvantitativné kysličník siřičitý a meá, pričom chulové a vonné látky destilátu nie sú ovplyvnené. Uvedeným postupom odstránia sa z destilátu spoTahlivo aj vysoké koncentrácie kysličníka siřičitého, 500 až 1 000 mg.l-1 i viac, ako aj vySěie koncentrácie médi. Súčasne odstránia sa aj koloidné a zákálové částice z destilátu.Using the method of the invention, the quantitative sulfur dioxide and melamine are removed from the distillate, while the flavorings of the distillate are not affected. High sulfur dioxide concentrations of 500 to 1000 mg.l -1 or more are also reliably removed from the distillate by this process, as well as higher media concentrations. At the same time, the colloidal and turbid particles are also removed from the distillate.
Vinny destilát, ako aj iné destiláty upravené spňsobom podTa vynálezuivyhóvia aj najprísnejgím kritériam na kvalitu, i pre vývoz do zahraničia.Wine distillate, as well as other distillates treated in accordance with the invention, also meets the strictest quality criteria, even for export abroad.
SpSsob podTa vynálezu mSže sa použiť v ktoromkoTvek Stádiu výroby destilátov. Ak sa použije pri úpravě tzv. surového destilátu před rektifikáciou, zabráni sa korozii destilačného zariadenia pri áalšej destilécii, číže rektifikácii, čím sa podstatné predíži životnost zariadenia.The process according to the invention can be used at any stage of the production of distillates. If it is used to modify the so-called. of crude distillate prior to rectification, corrosion of the distillation apparatus is prevented during further distillation, thus rectifying, thereby substantially extending the service life of the apparatus.
SpSsob podTa vynálezu mSže sa použiť a je vhodný pře vSetky ovocné a iné destiláty a najma v tých prípadoch, kde sa pri ogetrovaní kvasných substrátev používá kysličník siřičitý. MSže sa použiť aj při úprava niektorých kvasných substrátov.The method according to the invention can be used and is suitable for all fruit and other distillates and in particular in cases where sulfur dioxide is used in the fermentation of fermentation substrates. It can also be used in the treatment of some fermentation substrates.
Přiklad 1Example 1
Je potřebné upraviť vinny, alebo iný destilát, ktorý obsahuje 120 mg.'l-' kysličníka siřičitého, 11,0 mg.l-' médi a má pH 2,95.The adaptation cellar or other distillate containing 120 mg.'l - "carbon dioxide, 11.0 mg · l - 'copper and has a pH of 2.95.
Do destilátu sa 1,75 g.l-1 Ca(0H)2 přidá v 5 až 20% suspenzii, dokonale sa premiega, pričom sa upraví pH na 8,5 a prebehnú následovně reakoie:To the distillate, 1.75 gl -1 Ca (OH) 2 is added in a 5 to 20% suspension, mixed thoroughly, adjusting the pH to 8.5 and following the reaction:
H2SO3 + Ca (OH) 2->· CaSO3 . 2H2OH 2 SO 3 + Ca (OH) 2 -> · CaSO 3 . 2H 2 O
Cu2+ + Ca(OH)2 -> Cu(0H)2 + Ca2+ Cu 2+ + Ca (OH) 2 -> Cu (OH) 2 + Ca 2+
Pri týchto reakciach sa vápenaté soli vylučujú ako blelé zrazeniny příslušných siričitanov a alkalické hydroxidy dávajú s meánatými solami zrazeninu Cu(OH)2< Vyzráženie a vyčistenie destilátu sa podpoří uvedenými doplňujúcimi čeriacimi prostriedkami.In these reactions, the calcium salts precipitate as white precipitates of the respective sulfites and the alkali hydroxides give a precipitate of Cu (OH) 2 with the mesylated salts. The precipitation and purification of the distillate is aided by the above-mentioned additional blackening agents.
Po 24 hodinách sa destilát přetočí, alebo přefiltruje a přidá sa kyselina vinna v množstve 170 mg.l-', premiega a nechá sa reagovat 1 až 2 dni, pričom sa upraví pH na 4 a ro«2+ puštěný vápnik Ca v destiláte reaguje následovně.After 24 hours, the distillate rewind, and filtered, and treated with tartaric acid in an amount of 170 mg · l - ', premiega and treated 1-2 days, the pH was adjusted to 4 Bl' Ca 2+ released by calcium in the distillate is treated as follow.
♦♦
Ca2+ + C4H6O6 -> CaC4H4O6 Ca 2+ + C 4 H 6 O 6 -> CaC 4 H 4 O 6
Pri reakcii sa vyzráža víňan vápenatý, ktorý sa odstráni přetočením, alebo filtráciou.The reaction precipitates calcium tartrate, which is removed by rotation or filtration.
Stanovenie dávky vápenatéj suspenzie Ca(0H)2 Determination of Ca (OH) 2 calcium suspension
Do vzorky destilátu, ktorý sa má upraviť, přidává sa postupné 5 až 20% vápenatá suspenzia a titruje sa na fenolftalein do intenzívneho růžového sfarbenia.Add to the sample of distillate to be treated a sequential 5 to 20% calcium suspension and titrate to phenolphthalein until intense pink coloration.
Ak sa napr. na 25 ml destilátu spotřebuje 1,5 ml vápenatej suspenzie, potřebuje sa na 1 liter 60 ml rovnakej vápenatej suspenzie, alebo úměrně menšie množstvo Ca(0H)2, avšak nižšej koncentrácie.If, for example, per ml of distillate consumes 1.5 ml of calcium suspension, 60 ml of the same calcium suspension is needed per liter, or a proportionally smaller amount of Ca (OH) 2 , but a lower concentration.
Stanovenie dávky kyseliny vínnejDetermination of tartaric acid dose
Do 10 ml filtrátu po ošetření s Ca(0H)2 přidává sa 1%. roztok kyseliny vínnej, pričom reakcia sa sleduje pH - metrickou titráciou až do požadovaného pH (napr. 4,3).1% is added to 10 ml of the filtrate after treatment with Ca (OH) 2 . tartaric acid solution, the reaction being monitored by pH - titration up to the desired pH (e.g. 4.3).
Ak je spostreba napr. 0,16 ml, znamená to, že na 1 liter destilátu je potřebné 150 mg.I-' kyseliny vínnej,If the consumption is e.g. 0.16 ml, this means that for 1 liter of distillate was required 150 mg.l - "tartaric acid,
Príklad 2Example 2
Použije se postup ako v příklade 1, avšak miesto kyseliny vínnej použije sa iných kyselin, čím sa v prvej fáze vyzráža časť vápnika vo formě Ca-solí a zvyšok vápnika odstráni sa kyselinou vinnou vo formě vínanu vápenatého, čím sa aj upraví pH destilátu na požadovaná mieru.The procedure described in Example 1 is followed, but other acids are used instead of tartaric acid, whereby in the first stage some calcium is precipitated as Ca salts and the remaining calcium is removed by tartaric acid as calcium tartrate, thereby also adjusting the pH of the distillate to the desired peace.
P r í k 1 a d 3 ,Example 1, d 3,
Použije sa postup ako v příklade 1, avšak vápenatá suspenzia sa přidá do produktu po prvej destilácii, pričom sa odstráni kysličník siřičitý a meň. V produkte sa podTa potřeby » čiastočne upraví pH a prevedie sa rektifikácia. Kyselina vinna a iné kyseliny sa pridajú až do hotového rektifikovaného destilátu, čím sa odstránia zvyšky vápnika a zabráni sa vápenatým zákalom v destiláte, pričom sa súčasné upraví pH na požadovaná mieru.The procedure as in Example 1 is followed, but the calcium suspension is added to the product after the first distillation to remove sulfur dioxide and copper. The product is partially adjusted to pH and rectified as necessary. Tartaric acid and other acids are added to the finished rectified distillate to remove calcium residues and prevent calcium haze in the distillate while simultaneously adjusting the pH to the desired level.
Claims (2)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CS272880A CS211141B1 (en) | 1980-04-18 | 1980-04-18 | Method of removal of sulphur dioxyde,copper and colloidal turbid substances out from wine,fruit and other destillates |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CS272880A CS211141B1 (en) | 1980-04-18 | 1980-04-18 | Method of removal of sulphur dioxyde,copper and colloidal turbid substances out from wine,fruit and other destillates |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CS211141B1 true CS211141B1 (en) | 1982-01-29 |
Family
ID=5365194
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CS272880A CS211141B1 (en) | 1980-04-18 | 1980-04-18 | Method of removal of sulphur dioxyde,copper and colloidal turbid substances out from wine,fruit and other destillates |
Country Status (1)
| Country | Link |
|---|---|
| CS (1) | CS211141B1 (en) |
-
1980
- 1980-04-18 CS CS272880A patent/CS211141B1/en unknown
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