CS240348B1 - Method of d-xylose and l-arabinose preparation from maize ears - Google Patents
Method of d-xylose and l-arabinose preparation from maize ears Download PDFInfo
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- CS240348B1 CS240348B1 CS848079A CS807984A CS240348B1 CS 240348 B1 CS240348 B1 CS 240348B1 CS 848079 A CS848079 A CS 848079A CS 807984 A CS807984 A CS 807984A CS 240348 B1 CS240348 B1 CS 240348B1
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- xylose
- arabinose
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- 240000008042 Zea mays Species 0.000 title claims abstract description 13
- 235000002017 Zea mays subsp mays Nutrition 0.000 title claims abstract description 11
- 238000000034 method Methods 0.000 title claims abstract description 10
- 238000002360 preparation method Methods 0.000 title claims description 13
- 235000016383 Zea mays subsp huehuetenangensis Nutrition 0.000 title 1
- PYMYPHUHKUWMLA-VPENINKCSA-N aldehydo-D-xylose Chemical compound OC[C@@H](O)[C@H](O)[C@@H](O)C=O PYMYPHUHKUWMLA-VPENINKCSA-N 0.000 title 1
- PYMYPHUHKUWMLA-VAYJURFESA-N aldehydo-L-arabinose Chemical compound OC[C@H](O)[C@H](O)[C@@H](O)C=O PYMYPHUHKUWMLA-VAYJURFESA-N 0.000 title 1
- 210000005069 ears Anatomy 0.000 title 1
- 235000009973 maize Nutrition 0.000 title 1
- SRBFZHDQGSBBOR-UHFFFAOYSA-N beta-D-Pyranose-Lyxose Natural products OC1COC(O)C(O)C1O SRBFZHDQGSBBOR-UHFFFAOYSA-N 0.000 claims abstract description 33
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 24
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 22
- SRBFZHDQGSBBOR-IOVATXLUSA-N D-xylopyranose Chemical compound O[C@@H]1COC(O)[C@H](O)[C@H]1O SRBFZHDQGSBBOR-IOVATXLUSA-N 0.000 claims abstract description 17
- SRBFZHDQGSBBOR-HWQSCIPKSA-N L-arabinopyranose Chemical compound O[C@H]1COC(O)[C@H](O)[C@H]1O SRBFZHDQGSBBOR-HWQSCIPKSA-N 0.000 claims abstract description 16
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 14
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 12
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 claims abstract description 10
- 235000005822 corn Nutrition 0.000 claims abstract description 10
- 239000007864 aqueous solution Substances 0.000 claims abstract description 3
- 239000000243 solution Substances 0.000 claims description 14
- 230000007062 hydrolysis Effects 0.000 claims description 6
- 238000006460 hydrolysis reaction Methods 0.000 claims description 6
- 239000003814 drug Substances 0.000 abstract description 4
- 235000013305 food Nutrition 0.000 abstract description 3
- 239000002777 nucleoside Substances 0.000 abstract description 3
- 125000003835 nucleoside group Chemical group 0.000 abstract description 3
- 239000002773 nucleotide Substances 0.000 abstract description 3
- 125000003729 nucleotide group Chemical group 0.000 abstract description 3
- 239000011260 aqueous acid Substances 0.000 abstract 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 14
- 239000006188 syrup Substances 0.000 description 11
- 235000020357 syrup Nutrition 0.000 description 11
- 235000019441 ethanol Nutrition 0.000 description 8
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 6
- 150000002500 ions Chemical class 0.000 description 6
- 238000001816 cooling Methods 0.000 description 4
- 238000002425 crystallisation Methods 0.000 description 4
- 230000008025 crystallization Effects 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 3
- 230000003287 optical effect Effects 0.000 description 3
- 238000000967 suction filtration Methods 0.000 description 3
- 235000016068 Berberis vulgaris Nutrition 0.000 description 2
- 241000335053 Beta vulgaris Species 0.000 description 2
- 229920002488 Hemicellulose Polymers 0.000 description 2
- -1 aldopentose carbohydrates Chemical class 0.000 description 2
- 235000014633 carbohydrates Nutrition 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 238000005325 percolation Methods 0.000 description 2
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 description 2
- 229910052939 potassium sulfate Inorganic materials 0.000 description 2
- 235000011151 potassium sulphates Nutrition 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 229920001221 xylan Polymers 0.000 description 2
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 description 1
- 240000000731 Fagus sylvatica Species 0.000 description 1
- 235000010099 Fagus sylvatica Nutrition 0.000 description 1
- 229920001284 acidic polysaccharide Polymers 0.000 description 1
- 150000004805 acidic polysaccharides Chemical class 0.000 description 1
- 239000003929 acidic solution Substances 0.000 description 1
- 125000003277 amino group Chemical group 0.000 description 1
- PYMYPHUHKUWMLA-UHFFFAOYSA-N arabinose Natural products OCC(O)C(O)C(O)C=O PYMYPHUHKUWMLA-UHFFFAOYSA-N 0.000 description 1
- 150000001720 carbohydrates Chemical class 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 239000003610 charcoal Substances 0.000 description 1
- 239000003337 fertilizer Substances 0.000 description 1
- 235000013312 flour Nutrition 0.000 description 1
- 238000001640 fractional crystallisation Methods 0.000 description 1
- 239000003456 ion exchange resin Substances 0.000 description 1
- 229920003303 ion-exchange polymer Polymers 0.000 description 1
- 210000003127 knee Anatomy 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 150000002772 monosaccharides Chemical class 0.000 description 1
- 239000001120 potassium sulphate Substances 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
- 150000004823 xylans Chemical class 0.000 description 1
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- Saccharide Compounds (AREA)
Abstract
Podstata spósobu spočívá v tom, že sa 10 až 20 % hmot. hmota kukuřičných oklaskov predhydrolyzuje v 4 % hmot. vodnom roztoku kyseliny octovej pri teplote 100 °C po dobu 2 h, kde sa přednostně odhydrolyzuje L-arabinóza a zostávajúca hmota sa hydrolyzuje 1 % hmot. vodným roztokom kyseliny sírovej pri teplote 100 °C po dobu 4 až 6 h za odhydrolyzovania D-xy.lózy a jednotlivé hydrolyzáty sa prečistia aktívnym uhlím a vykrystalizuji! z etanolu. Vynález má rozsiahle použitie v potravinárskom priemysle v biochemii, v medicíně, ako aj pri přípravě nových nukleozidov a nukleotidov, ktoré majú použitie- v bioinžinierstve.The essence of the method is that 10 % to 20 wt. mass of corn cobs prehydrolysed at 4 wt. aqueous solution acetic acid at 100 ° C after for 2 h, where it is preferably hydrolyzed L-arabinose and the remaining mass are hydrolyzed 1 wt. aqueous acid sulfuric acid at 100 ° C for 4 to 4 hours 6 h with dehydrolysis of D-xylose and single the hydrolysates are purified with activated carbon and I crystallize! from ethanol. The invention has extensive use in the food industry in biochemistry, medicine, as well as in medicine preparing new nucleosides and nucleotides, which are used in bioengineering.
Description
(54) Sposob přípravy D-xyíúzy a L-arabinózy z kukuřičných oklaskov(54) Method of preparation of D-xylose and L-arabinose from corn cob
ŽFROM
Podstata spósobu spočívá v tom, že sa 10 až 20 % hmot. hmota kukuřičných oklaskov predhydrolyzuje v 4 % hmot. vodnom roztoku kyseliny octovej pri teplote 100 °C po dobu 2 h, kde sa přednostně odhydrolyzujeThe essence of the method is that 10 to 20 wt. the mass of corn cob prehydrolyses in 4 wt. aqueous acetic acid solution at 100 ° C for 2 h, where it is preferably dehydrolyzed
L-arabinóza a zostávajúca hmota sa hydrolyzuje 1 % hmot. vodným roztokom kyseliny sírovej pri teplote 100 °C po dobu 4 až h za odhydrolyzovania D-xy.lózy a jednotlivé hydrolyzáty sa prečistia aktívnym uhlím a vykrystalizuji! z etanolu. Vynález má rozsiahle použitie v potravinárskom priemysle v biochemii, v medicíně, ako aj pri přípravě nových nukleozidov a nukleotidov, ktoré majú použitie- v bioinžinierstve.L-arabinose and the remaining mass are hydrolyzed with 1 wt. aqueous sulfuric acid solution at 100 ° C for 4 to h while dehydrolyzing the D-xylose and the individual hydrolyzates are purified with activated carbon and crystallized! of ethanol. The invention has extensive application in the food industry in biochemistry, medicine, as well as in the preparation of novel nucleosides and nucleotides to be used in bioengineering.
Vynález sa týká sposobu přípravy kryštallckej D-xylózy a krystalické]' L-arabinózy z kukuřičných oklaskov.The invention relates to a process for the preparation of crystalline D-xylose and crystalline L-arabinose from corn cob.
D-xylúza ako aj L-arabinóza patria medzi vzácné sacharidy aldopentózy. V prírode sa vol'ne nachádzajú zriedka, častejšie vo forjne derivátov, alebo polymérnych sacharidov. V důsledku ich stále vačšieho praktického použitia sa ich príprave venuje zvýšená pozornost a zároveň sa híadajú nové netradičné zdroje surovin. Na výrobu D-xylózy sa doteraz používajú přírodně materiály ako bukové štiepky, piliny pomocou hydrolýzy, alebo hydrolýzou xylanov a hemicelulóz [W. E. Stone, D. Lotz: J. Am. Chem. 13, 348 (1891); W. E. Stone, D. Lotz: Chem. News. 64, 29 (1891); W. E. Stone, D. Lotz: Ghemiche Ber. 24, 1657 (1981); W. T. Scheiber, N. V. Geib, B. Wingfield, S. F. Acree: Ind. Eng. Chem. 22, 497 (1930); C. S. Hudson, T. S. Harding: J. Am. Chem. Soc. 40, 1 601 (1981)]. L-arabinóza sa vyrába parciálnou hydrolýzou gúm róznych dřevin a následnou frakčnou kryštalizáciou vzniklej zmesi (E. Anderson, L. Sands: Org. syntheses. 8, 18 (1929); E. W. White: J. Am. Chem. Soc. 69, 715 (1947); C. S. Hudson: J. Am. Chem. Soc. 73, 4 038 (1951); J. Rosík, V. Zitko, Š. Bauer, J. Kubala: Collection Czechoslov. Commun. 31, 1 072 (1966)). V. Tibenský připravil L-arabinózu z vysladených repných rezkov [Čs. A. O. 129 664, A. O. 139 427], Uvedené metody přípravy D-xylózy z dřevných štiepkov, pilin alebo hydrolýzou xylanov hemicelulóz sa v praxi používajú, avšak sú nákladné na energiu. Příprava L-arabinózy parciálnou hydrolýzou gúm dřevin sa v praxi nevyužívá. Pri príprave z vysladených repných rezkov vznikajú koloidné zložky alebo kyslé polysacharidy a na ich odstránenie sa požaduje speciálně zariadenie, čím sa příprava stává nákladnou na zariadenie.D-xylose and L-arabinose are rare aldopentose carbohydrates. They are rarely found in nature, more often in the form of derivatives or polymeric carbohydrates. As a result of their increasing practical application, their preparation is given increased attention and new non-traditional sources of raw materials are being sought. Until now, natural materials such as beech chips, sawdust by hydrolysis, or hydrolysis of xylanes and hemicelluloses have been used to produce D-xylose [W. E. Stone, D. Lotz, J. Am. Chem. 13, 348 (1891); W.E. Stone, D. Lotz: Chem. News. 64, 29 (1891); W.E. Stone, D. Lotz: Ghemiche Ber. 24, 1657 (1981); W. T. Scheiber, N.V. Geib, B. Wingfield, S.F. Acree: Ind. Eng. Chem. 22, 497 (1930); Hudson C. S. Harding T. Am. Chem. Soc. 40, 1601 (1981)]. L-arabinose is produced by partial hydrolysis of gums of different woody species and subsequent fractional crystallization of the resulting mixture (E. Anderson, L. Sands: Org. Syntheses. 8, 18 (1929); EW White: J. Am. Chem. Soc. 69, 715) (1947) CS Hudson: J. Am. Chem Soc., 73, 4 038 (1951), J. Rosik, V. Zitko, S. Bauer, J. Kubala: Collection Czech and Slovak Commun., 31, 1072 (1966) )). V. Tibenský prepared L-arabinose from sweetened beet pulp [Čs. A. O. 129 664, A. O. 139 427], The methods for the preparation of D-xylose from wood chips, sawdust or xylan hydrolysis of hemicelluloses are used in practice, but are expensive for energy. The preparation of L-arabinose by partial hydrolysis of woody gums is not used in practice. In the preparation of the sweetened beet pulp, colloidal components or acidic polysaccharides are produced and a special device is required to remove them, making the preparation expensive for the device.
Uvedené nevýhody v podstatnej miere odstraňuje spósob přípravy D-xylózy a L-arabinózy, ktorého podstata spočívá v tom, že sa 10 až 20 % hmot. pomletých kukuřičných oklaskov predhydrolyzuje v 4 % hmot. vodnom roztoku kyseliny octovej pri teplote 100 °C po dobu 2 h, kde sa přednostně odhydrolyzuje L-arabinóza a zostávajúca hmota sa hydrolyzuje 1% hm. vodným roztokom kyseliny sírovej pri teplote 100 °C po dobu 4 až 6 h za odhydrolyzovania D-xylózy a jednotlivé hydrolyzáty sa prečistia aktívnym uhlím a vykryštalizujú z etanolu.The above-mentioned disadvantages are substantially eliminated by the process for the preparation of D-xylose and L-arabinose, which consists in the fact that 10 to 20 wt. ground corn cob prehydrolyzed in 4 wt. of an aqueous acetic acid solution at 100 ° C for 2 h, wherein preferably L-arabinose is dehydrolyzed and the remaining mass is hydrolyzed with 1 wt. aqueous sulfuric acid solution at 100 ° C for 4-6 hours with dehydrolysis of D-xylose, and the individual hydrolysates are purified by charcoal and crystallized from ethanol.
Výhodou navrhovaného spósobu přípravy D-xylózy a L-arabinózy z kukuřičných oklaskom oproti doterajším postupom přípravy je, že předmětný spósob přípravy je jednoduchší, hospodárnější a účinnější. Dovoluje pracovat v nenáročných jednoduchých zarladeniach. Umožňuje vyrobit z lacnej nenáročnej suroviny obidva monosacharidy, ktoré sú krystalické látky o vysokej čistotě. Pri výrobě odpadne látky neznečisťujú prostredie, ale sa používajú ako účinné hnojivo.The advantage of the proposed process for the preparation of D-xylose and L-arabinose from maize corns over the prior art is that the process is simpler, more economical and more efficient. It allows to work in undemanding simple devices. It makes it possible to make both monosaccharides, which are crystalline substances of high purity, from a cheap, undemanding raw material. In production, waste materials do not pollute the environment, but are used as an effective fertilizer.
Příklad 1Example 1
K roztoku (250 g) pomletých kukuřičných oklaskov v (4,7 1) vody sa přidá (300 ml) kyseliny octovej 100 % hmot. a mieša sa pri teplote 100 °C po dobu 2 h. Po ochladení sa roztok oddělí od hmoty filtráciou na nuči, premyje vodou (2 1] a zahustí pri tlaku —100 KPa za súčasného odstránenia kyseliny octovej. Roztok sa přečistí prídavkom aktívneho uhlia (10 g), přefiltruje a perkoluje cez ionomenič s funkčnými sulf osk upinami (Wofatit KPS 200] v hydrogénovej formě na kolóne s dížkou 30 cm a priemerom 3 cm a ionomenič s funkčnou amínoskupinou ( Wofatit SBW) v hydroxidovéj formě na kolóne s dížkou 50 cm a priemerom 3 cm a sa zahustí na sirup (25%). Sirup sa rozpustí v 96 % hmot. etylalkohole a vykrystalizuje (9,6 g), opakovanou kryštalizáciou matečných lúhov sa získá dalších (3,15 g) L-ara binózy v celkovom výtažku 5,1 %, optická otáčavosť [alf,20 —104 (C — 5 voda), teplota topenia 162 °C. Predhydrolyzované kukuřičné oklasky sa ďalej hydrolyzujú prídavkom vody (4,87 1) a kyseliny sírové] 96 pere. hmot. (135 ml) a refluxujú za miešania po dobu 6 h pri teplote 100 °C. Reakčná zmes sa filtráciou na nuči zbaví celulózových zvyškov a balastov a neutralizuje prídavkom krystalického hydroxidu draselného (300 g) a zahustí pri tlaku —100 KPa na sirup (130 g). Zmes sa mieša prídavkom 50 pere. hmot. vodného etylalkoholu (0,5 1) pri teplote 40 °C po dobu 1 h. Po ochladení vykryštalizuje síran draselný, ktlorý sa oddělí filtráciou. Roztok sa pri tlaku —100 KPa zahustí na sirup, přečistí prídavkom aktívneho uhlia (10 g), přefiltruje a odsolí perkoláciou cez ionomenič s funkčnou sulfoskupinou (Wofatit KPS 200) v hydrogénovej formě na kolóne s dížkou 50 cm a priemerom 3 cm a ionomenič s funkčnou amínoskupinou (Wofatit SBW) v hydroxidovej formě na kolóne s dížkou 50 cm a priemerom 3 cm, zahustí na sirup (71 g). Sirup sa rozpustí v 96 % hmot. etylalkohole (100 ml) pri teplote 78°C a vykryštalizuje D-xylózy (46 g). Opakovanou kryštalizáciou matečných lúhov sa získá D-xylóza v 20,3 % výtažku, optická otáčavosť [a]D 20 +20° (G = 5 voda), teplota topenia 147 °C.To a solution (250 g) of ground corn flour in (4.7 L) water was added (300 mL) 100% acetic acid. and stirred at 100 ° C for 2 h. After cooling, the solution was separated from the mass by suction filtration, washed with water (2 L) and concentrated at 100100 KPa while removing acetic acid.The solution was purified by addition of activated carbon (10 g), filtered and percolated through a functional sulfonic acid ion exchanger. Upins (Wofatit KPS 200) in hydrogen form on a 30 cm 3 cm diameter column and an amine-functional ion exchanger (Wofatit SBW) in hydroxide form on a 50 cm 3 cm diameter column and concentrated to a syrup (25%) The syrup is dissolved in 96% ethyl alcohol and crystallized (9.6 g), by repeated crystallization of the mother liquors to give an additional (3.15 g) of L-ara binose in a total yield of 5.1%, optical rotation [alpha, 20, 162 (C-5 water), melting point 162 DEG C. The prehydrolyzed corn cob is further hydrolyzed by the addition of water (4.87 L) and sulfuric acid (96 ml) (135 ml) and refluxed with stirring for 6 h. at 100 ° C the mixture was filtered under suction and the residue freed from cellulose ballast and neutralized by the addition of crystalline potassium hydroxide (300 g) and evaporated at a pressure of -100 kPa to a syrup (130 g). The mixture was stirred by the addition of 50 pens. wt. aqueous ethyl alcohol (0.5 L) at 40 ° C for 1 h. After cooling, potassium sulphate crystallizes and is separated by filtration. The solution is concentrated to a syrup at a pressure of 100100 KPa, clarified by the addition of activated carbon (10 g), filtered and desalinated by percolation through a sulfofunctional ion exchanger (Wofatit KPS 200) in hydrogen form on a 50 cm 3 cm diameter column and ion exchanger. A functionalized amino group (Wofatit SBW) in hydroxide form on a 50 cm 3 cm diameter column, concentrated to a syrup (71 g). The syrup is dissolved in 96 wt. ethyl alcohol (100 mL) at 78 ° C and crystallized D-xylose (46 g). Repeated crystallization of the mother liquors gave D-xylose in 20.3% yield, optical rotation [α] D 20 + 20 ° (G = 5 water), mp 147 ° C.
Příklad 2Example 2
K roztoku (200 kg) pomletých kukuřičných oklaskov (800 1) vody sa přidá (40 kilogramov) kyseliny octovej 100% hmot. a mieša pri teplote 100 °C po dobu 2 h. Po ochladení sa roztok od hmoty oddělí filtráciou na nuči, premyje vodou (200 lj a.zahustí pri tlaku —100 KPa za súčasného odstránenia kyseliny octovej. Roztok sa přečistí prídavkom aktívneho uhlia (2 kg), přefiltruje a perkoluje cez ionomenič s funkčnou sulfoskupinou (Wofatit KPS 200) v hydrogénovej formě na kolene s dížkou 1 meter a priemerom 0,2 m a ionoinenič s funkčnou amínoskupinou (Wofatit SBW) v hydroxidovej formě s dížkou kolony 1 m a priemerom 0,2 m, zahustí na sirup (15 kg). Sirup sa rozpustí v (20 1) 86% hmot. etylalkohole pri teplote 78 °C a .vykrystalizuje (7,8 kg) L-arabinózy. Opakovanou kryštalizáciou sa získá dalších (3,2 kg) L-arabinózy. L-arabinóza mala optickú otáčavosf [;«)D 20 —104° (C = 5 voda), teplotu topenia 162 °C a sa získala v 5,5 °/o výtažku. Predhydrolyzované kukuřičné oklasky sa dále] hydrolyzujú tak, že sa přidá (800 1) vody, (20 1) kyseliny sírovej 98 % hmot. a refluxujú za miešania prii teplote 100 °C podobu 4 h. Kyslý roztok po filtrácii na nuči sa neutralizuje prídavkom krystalického hydroxidu draselného (4,2 kg) a odpaří pri tlaku —100 KPa na sirup (100 1). Táto zmes sa nheša prídavkom 50 °/o hmot. vodného roztoku etylalkoholu (400 1) pri teplote 40° Celsia po dobu 1 h. Po ochladení vykryštalizuje síran draselný, ktorý sa oddělí filtráciou. Roztok sa zahustí na sirup, přečistí prídavkom aktívneho uhlia (2 kg), přefiltruje a odsolí perkoláciou cez ionomenič s funkčnou sulfoskupinou (Wofatit KPS 200) v hydrogénovej formě na kolóne s dížkou 2 m a priemerom 0,3 m a ionomenič s funkčnou amínoskupinou (Wofatit SBWj v hydroxidové) formě na kolóne s dížkou 2 m a priemerom 0,3 m, zahustí na sirup (100 kg). Sirup sa rozpustí v 96 % hmot. etylalkohole (100 1) pri teplote 78 °C a v chladiacom boxe pri teplote 5 °C vykrystalizuje D-xylóza (36 kg). Opakovanou kryštalizáciou sa získá dalších (6 kg) D-xylózy. D-xylóza mala optickú otáčavost [aji-,20 + 20p (C = 5 voda), teplotu topenia 146 až 148 °C a získala sa v 21 % výtažku.To a solution (200 kg) of ground corn cob (800 L) water (40 kg) of acetic acid 100 wt. and stirred at 100 ° C for 2 h. After cooling, the solution is separated from the mass by suction filtration, washed with water (200 µl and concentrated at 100100 kPa while removing acetic acid. The solution is purified by addition of activated charcoal (2 kg), filtered and percolated through a sulfo-functional ion exchanger ( Wofatit KPS 200) in hydrogen form on a knee of 1 meter length and 0.2 m diameter and amine-functional ion exchange resin (Wofatit SBW) in hydroxide form with a column length of 1 m and 0.2 m diameter, thicken to a syrup (15 kg). Dissolve in (20 L) 86% ethyl alcohol at 78 ° C and crystallize (7.8 kg) of L-arabinose to give an additional (3.2 kg) of L-arabinose by repeated crystallization. [.alpha.] D @ 20 -104 DEG (C = 5 water), m.p. 162 DEG C. and obtained in 5.5% of the yield. The prehydrolyzed corn cob is further hydrolyzed by adding (800 L) water, (20 L) sulfuric acid 98 wt. and reflux with stirring at 100 ° C for 4 h. The acidic solution after suction filtration is neutralized by addition of crystalline potassium hydroxide (4.2 kg) and evaporated at a pressure of -100 KPa to a syrup (100 L). This mixture is quenched by the addition of 50% w / w. of an aqueous solution of ethyl alcohol (400 L) at 40 ° C for 1 h. Upon cooling, potassium sulfate crystallizes and is collected by filtration. The solution is concentrated to a syrup, clarified by the addition of activated carbon (2 kg), filtered and desalinated by percolation through a sulfo-functional ion exchanger (Wofatit KPS 200) in a hydrogenated form on a 2 m long column and 0.3 m diameter amine-functional ion exchanger (Wofatit SBWj in hydroxide form on a column 2 m long and 0.3 m diameter, thicken to a syrup (100 kg). The syrup is dissolved in 96 wt. Ethyl alcohol (100 L) at 78 ° C and D-xylose (36 kg) crystallized in a 5 ° C refrigerator. Repeated crystallization gave an additional (6 kg) D-xylose. D-xylose had an optical rotation [α], 20 + 20 µ (C = 5 water), mp 146-148 ° C and was obtained in 21% yield.
Vynález má rozsiahle použitie v potravinářském priemysle v biochemii, medicíně, ako aj při príprave nových nukleozidov a nukleotidov, ktoré majú použitie v bioinžinierstve.The invention has extensive application in the food industry in biochemistry, medicine, as well as in the preparation of novel nucleosides and nucleotides for use in bioengineering.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CS848079A CS240348B1 (en) | 1984-10-24 | 1984-10-24 | Method of d-xylose and l-arabinose preparation from maize ears |
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| Application Number | Priority Date | Filing Date | Title |
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| CS848079A CS240348B1 (en) | 1984-10-24 | 1984-10-24 | Method of d-xylose and l-arabinose preparation from maize ears |
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| CS807984A1 CS807984A1 (en) | 1985-06-13 |
| CS240348B1 true CS240348B1 (en) | 1986-02-13 |
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| CS848079A CS240348B1 (en) | 1984-10-24 | 1984-10-24 | Method of d-xylose and l-arabinose preparation from maize ears |
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