CS244591B1 - Xylanes preparation method from one year's plants - Google Patents
Xylanes preparation method from one year's plants Download PDFInfo
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- CS244591B1 CS244591B1 CS85395A CS39585A CS244591B1 CS 244591 B1 CS244591 B1 CS 244591B1 CS 85395 A CS85395 A CS 85395A CS 39585 A CS39585 A CS 39585A CS 244591 B1 CS244591 B1 CS 244591B1
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- aqueous
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- hydroxide solution
- alcohol
- xylans
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- 229920001221 xylan Polymers 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title abstract description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 24
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 20
- 150000004823 xylans Chemical class 0.000 claims abstract description 16
- 239000000463 material Substances 0.000 claims abstract description 9
- 239000000284 extract Substances 0.000 claims abstract description 8
- ZKQDCIXGCQPQNV-UHFFFAOYSA-N Calcium hypochlorite Chemical compound [Ca+2].Cl[O-].Cl[O-] ZKQDCIXGCQPQNV-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000005406 washing Methods 0.000 claims abstract description 5
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000000460 chlorine Substances 0.000 claims abstract description 4
- 229910052801 chlorine Inorganic materials 0.000 claims abstract description 4
- 238000001556 precipitation Methods 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 13
- 239000007800 oxidant agent Substances 0.000 claims description 6
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 5
- 239000005708 Sodium hypochlorite Substances 0.000 claims description 5
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 claims description 4
- 239000000126 substance Substances 0.000 abstract description 5
- 235000013305 food Nutrition 0.000 abstract description 4
- 239000004753 textile Substances 0.000 abstract description 2
- 239000003153 chemical reaction reagent Substances 0.000 abstract 2
- WQYVRQLZKVEZGA-UHFFFAOYSA-N hypochlorite Chemical compound Cl[O-] WQYVRQLZKVEZGA-UHFFFAOYSA-N 0.000 abstract 2
- 230000001590 oxidative effect Effects 0.000 abstract 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 abstract 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 abstract 1
- 239000000654 additive Substances 0.000 abstract 1
- 230000000996 additive effect Effects 0.000 abstract 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 abstract 1
- 239000011591 potassium Substances 0.000 abstract 1
- 229910052700 potassium Inorganic materials 0.000 abstract 1
- 239000011734 sodium Substances 0.000 abstract 1
- 229910052708 sodium Inorganic materials 0.000 abstract 1
- 239000005418 vegetable material Substances 0.000 abstract 1
- 241000196324 Embryophyta Species 0.000 description 13
- SRBFZHDQGSBBOR-IOVATXLUSA-N D-xylopyranose Chemical compound O[C@@H]1COC(O)[C@H](O)[C@H]1O SRBFZHDQGSBBOR-IOVATXLUSA-N 0.000 description 11
- SRBFZHDQGSBBOR-UHFFFAOYSA-N beta-D-Pyranose-Lyxose Natural products OC1COC(O)C(O)C1O SRBFZHDQGSBBOR-UHFFFAOYSA-N 0.000 description 11
- PYMYPHUHKUWMLA-UHFFFAOYSA-N arabinose Natural products OCC(O)C(O)C(O)C=O PYMYPHUHKUWMLA-UHFFFAOYSA-N 0.000 description 9
- 235000019441 ethanol Nutrition 0.000 description 9
- PYMYPHUHKUWMLA-WDCZJNDASA-N arabinose Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)C=O PYMYPHUHKUWMLA-WDCZJNDASA-N 0.000 description 4
- 238000000605 extraction Methods 0.000 description 4
- 229920002488 Hemicellulose Polymers 0.000 description 3
- 240000008042 Zea mays Species 0.000 description 3
- 235000002017 Zea mays subsp mays Nutrition 0.000 description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 description 2
- 235000013339 cereals Nutrition 0.000 description 2
- 235000005822 corn Nutrition 0.000 description 2
- 239000010903 husk Substances 0.000 description 2
- 238000002955 isolation Methods 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 239000010902 straw Substances 0.000 description 2
- 239000002028 Biomass Substances 0.000 description 1
- 102000004190 Enzymes Human genes 0.000 description 1
- 108090000790 Enzymes Proteins 0.000 description 1
- SRBFZHDQGSBBOR-HWQSCIPKSA-N L-arabinopyranose Chemical compound O[C@H]1COC(O)[C@H](O)[C@H]1O SRBFZHDQGSBBOR-HWQSCIPKSA-N 0.000 description 1
- 241000209140 Triticum Species 0.000 description 1
- 235000021307 Triticum Nutrition 0.000 description 1
- 235000016383 Zea mays subsp huehuetenangensis Nutrition 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 150000001720 carbohydrates Chemical class 0.000 description 1
- 238000010908 decantation Methods 0.000 description 1
- 239000003599 detergent Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000000909 electrodialysis Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 239000008394 flocculating agent Substances 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 235000009973 maize Nutrition 0.000 description 1
- HEBKCHPVOIAQTA-UHFFFAOYSA-N meso ribitol Natural products OCC(O)C(O)C(O)CO HEBKCHPVOIAQTA-UHFFFAOYSA-N 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- HEBKCHPVOIAQTA-SCDXWVJYSA-N xylitol Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)CO HEBKCHPVOIAQTA-SCDXWVJYSA-N 0.000 description 1
- 235000010447 xylitol Nutrition 0.000 description 1
Landscapes
- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
Riešenie sa týká sposohu přípravy xylánov z jednoročných rastlín. Podstata přípravy spočívá v tom, že sa nastlinný materiál extrahuje 1 až 10 °/o hmot. vodným roztokom hydroxidu sodného alebo 3 až 24 % hmot. vodným roztokom hydroxidu draselného s přísadou oxidačného činidla v množstve, ekvivalentnom do 30 °/o hmot. aktívneho chlóru, vztahované na rastlinný materiál, pri teplote 25 až 80 °C po dobu 1 až 6 hodin a z alkalického extraktu sa xylány izolujú zrážaním v dvoj- až trojnásobnom objemovom množstve alkoholu a purifikujú premývaním s 70 až 85 % obj. vodným roztokom alkoholu. Ako oxidačně činidlo sa použije vodný roztok chlornanu sodného, alebo vodný roztok chlornanu vápenatého. Riešenie má použitie v priemysle celulózo-papierenskom, chemickom, potravinárskom, farmaceutickom a textilnom.The solution concerns the preparation of xylans of annual plants. The essence of the preparation lies in the fact that the lining material extracts 1 to 10% by weight. aqueous sodium hydroxide solution; \ tor. \ t 3 to 24 wt. aqueous hydroxide solution of potassium with an oxidizing additive reagents in an amount equivalent to 30% wt. active chlorine, related to vegetable material, at 25 to 80 ° C after for 1 to 6 hours and from an alkaline extract the xylans are isolated by precipitation in two to three times volume of alcohol; \ tand. \ t purify by washing with 70-85% vol. aqueous alcohol. As oxidative the reagent is an aqueous hypochlorite solution sodium or aqueous calcium hypochlorite solution. The solution is used in the pulp and paper industry, chemical, food, pharmaceutical and textile.
Description
(54) Sposob přípravy xylánov z jednoročných rastlín(54) Method for preparing xylans from annual plants
22
Riešenie sa týká sposohu přípravy xylánov z jednoročných rastlín.The solution concerns how to prepare xylans from annual plants.
Podstata přípravy spočívá v tom, že sa nastlinný materiál extrahuje 1 až 10 °/o hmot. vodným roztokom hydroxidu sodného alebo 3 až 24 % hmot. vodným roztokom hydroxidu draselného s přísadou oxidačného činidla v množstve, ekvivalentnom do 30 °/o hmot. aktívneho chlóru, vztahované na rastlinný materiál, pri teplote 25 až 80 °C po dobu 1 až 6 hodin a z alkalického extraktu sa xylány izolujú zrážaním v dvoj- až trojnásobnom objemovom množstve alkoholu a purifikujú premývaním s 70 až 85 % obj. vodným roztokom alkoholu. Ako oxidačně činidlo sa použije vodný roztok chlornanu sodného, alebo vodný roztok chlornanu vápenatého.The essence of the preparation consists in extracting the overlay material from 1 to 10% by weight. % aqueous sodium hydroxide solution or 3 to 24 wt. aqueous potassium hydroxide solution with oxidizing agent added in an amount equivalent to 30% w / w. of active chlorine, based on plant material, at 25 to 80 ° C for 1 to 6 hours and from the alkaline extract, xylanes are isolated by precipitation in two to three times the volume of alcohol and purified by washing with 70 to 85% v / v. aqueous alcohol solution. As the oxidizing agent, an aqueous sodium hypochlorite solution or an aqueous calcium hypochlorite solution is used.
Riešenie má použitie v priemysle celulózo-papierenskom, chemickom, potravinárskom, farmaceutickom a textilnom.The solution is used in the pulp, paper, chemical, food, pharmaceutical and textile industries.
Vynález sa týká spůsobu přípravy xylánov z jednoročných rastlín.The invention relates to a process for preparing xylans from annual plants.
Heimicelulózy D-xylánového typu s různým obsahom L-arabinózy a urónových kyselin sú přítomné vo vláknitých častiach jednoročných rastlín v množstve 15 až 35 %. Tieto zdroje xylánov predstavujú v prevažnej miere odpady, vznikajúce pri spracovaní různých obilnin a iných pofnohospodárskych rastlín (slama, otruby, šupky kukuřičných zrn, kukuřičné vretená, šúpolie, palice ta pod.). Izoláciou hemicelulóz z jednoročných rastlín sa zaoberajú různé postupy, zahřňujúce zložitý komplex operácií, ako je úprava extrakciou, enzýmovým působením, delignifikáciou, viacstupňová extrakcia a purifikácia izolovaných hemicelulóz [K. C. B. Wilkie: Adv. Carbohydrate Chem. Biochem. 36, 215 (1979J; US pat. č. 4181796; US pat. 4 038 481; US ptat. číslo 4 017 642],D-xylan-type heimicelluloses with varying levels of L-arabinose and uronic acids are present in the fiber parts of annual plants in an amount of 15 to 35%. These xylan sources are predominantly wastes arising from the processing of various cereals and other agricultural plants (straw, bran, maize grain husks, corn spindles, husks, sticks, etc.). The isolation of hemicelluloses from annual plants is dealt with by a variety of procedures involving a complex complex of operations such as treatment by extraction, enzyme treatment, delignification, multi-stage extraction and purification of isolated hemicelluloses [K. Wilkie C. B.: Adv. Carbohydrate Chem. Biochem. 36, 215 (1979J; US Pat No. 4181796; US Pat. 4,038,481; US Pat. No. 4,017,642],
Izolácia xylánov týmito postupmi je náročná nielen na chemikálie, ale aj na energiu a technické zariadenia (vymrazovanie, elektrodialýza, tlakové posotaenie za vysokých teplůt), čo nepriaznivo ovplyvňuje ekonomiku výrobného procesu.The isolation of xylans by these processes is demanding not only for chemicals, but also for energy and technical equipment (freezing, electrodialysis, pressure swelling at high temperatures), which adversely affects the economics of the production process.
Uvedené nevýhody v podstatnej miere odstraňuje sposob přípravy xylánov z jednoročných rastlín podl'a vynálezu, ktorého podstata spočívá v tom, že sa rastlinný materiál extrahuje 1 až 10 % hmot. vodným roztokom hydroxidu sodného, alebo 3 až 24 % hmot. vodným roztokom hydroxidu draselného s přísadou oxidačného činidla v množstve, ekvivalentnom 0 až 30 % hmot. aktívneho chlóru, vztahované na rastlinný materiál. Ako oxidačně činidlo sa použije vodný roztok chlornanu sodného alebo vodný roztok chlornanu vápenatého pri teplote 25 až 80 °C, po dobu 1 až 6 hodin. Z alkalického extraktu sa xylány izolujú zrážaním v dvojaž trojnásobnom objemovom množstve alkoholu a purifikujú premývaním so 70 až 85 % obj. vodným roztokom alkoholu.The above-mentioned disadvantages are substantially eliminated by the process of preparing xylans from the annual plants according to the invention, which consists in extracting the plant material from 1 to 10% by weight. % aqueous sodium hydroxide solution, or 3 to 24 wt. % aqueous potassium hydroxide solution with an oxidizing agent added in an amount equivalent to 0 to 30 wt. active chlorine, based on plant material. An aqueous sodium hypochlorite solution or an aqueous calcium hypochlorite solution at 25 to 80 ° C for 1 to 6 hours is used as the oxidizing agent. From the alkaline extract, xylanes are isolated by precipitation in two to three times the volume of alcohol and purified by washing with 70 to 85% v / v. aqueous alcohol solution.
Výhodou navrhovaného postupu přípravy xylánov z jednoročných rastlín oproti známým postupom přípravy je, že předložený spůsob je ekonomicky efektivnější, pretože v jednom extrakčnom stupni sa izolujú D-xylány s vysokou čistotou vo výťažkoch 50 až 90 % z povodně přítomných hemicelulóz. Postup je tiež menej náročný na použité chemikálie, čas, energiu a prevádzkové zariadenie. Extrakčný zvyšok představuje celulózový materiál, vhodný na skřmovanie, alebo přípravu křmnej biomasy.The advantage of the proposed process for the preparation of xylans from annual plants over the known processes is that the present process is more economically efficient since high purity D-xylanes are isolated in one extraction stage in yields of 50 to 90% of the hemicelluloses present in the flood. The process is also less demanding on the chemicals used, time, energy and equipment. The extraction residue is a cellulosic material suitable for feeding or preparing feed biomass.
Příklad 1Example 1
Suspenzia 1,1 kg vzduchosuchej drtě kukuřičných vretien v 7,5 1 5 % hmot. vodného roztoku hydroxidu sodného sa za miešania zahřeje na teplotu 40 °C a udržuje pri tejto teplote po dobu 2 h. Potom sa extrakt odfiltruje cez sklenú tkaninu a k extrakčnému zvyšku sa přidá na premývanie 7,5 1 5 %-ného hmot. vodného roztoku hydroxidu sodného. Spojené extrakty sa zrážajú do 30 1 96 % obj. etylalkoholu. Rýchlo sedimentujúca zrazenina sa po druhej dekantácii v 70 % obj. etylalkohole neutralizuje zriedeným roztokom kyseliny octovej alebo sírovej a dalej premyje 70 až 85 % obj. zregenerovaným etylalkoholom až do· bezfarebného filtrátu. Po odvodnění zrazeniny xylánu 96 % obj. etylalkoholom sa získá xylán vo výtažku 30 % (vztahovaném na rastlinný materiál), ktorý obsahuje 93 % hmot. xylózy a arabinózy v mólovom pomere 1: 0,1.A suspension of 1.1 kg of air-dried pulp of corn spindles in 7.5 l of 5 wt. of aqueous sodium hydroxide solution is stirred and heated to 40 ° C with stirring for 2 h. The extract is then filtered through a glass cloth and 7.5% of 5% by weight is added to the extract residue for washing. aqueous sodium hydroxide solution. The combined extracts precipitated to 30% by volume. ethanol. The rapidly sedimenting precipitate was recovered at 70% v / v after the second decantation. neutralized with a dilute acetic or sulfuric acid solution and further washed with 70 to 85 vol. recovered with ethyl alcohol until a colorless filtrate. After draining the xylan precipitate, 96% by volume. with ethyl alcohol, xylan was obtained in a yield of 30% (based on plant material) containing 93% by weight. xylose and arabinose at a molar ratio of 1: 0.1.
Příklad 2Example 2
Postupuje sa ako v příkladu 1 s tým rozdielom, že sa použije 10 1 1 %-ného vodného roztoku hydroxidu sodného s prídavkom 700 ml 15 %-ného vodného roztoku chlornanu sodného pri 80 °C po dobu 1 h. Získá sa 19 % xylánu s obsahom 91 % hmot. xylózy a larabinózy v mólovom pomere 1: 0,15.The procedure is as in Example 1 except that 10 l of a 1% aqueous sodium hydroxide solution is added with the addition of 700 ml of a 15% aqueous sodium hypochlorite solution at 80 ° C for 1 h. 19% xylan is obtained with a content of 91% by weight. xylose and larabinose at a molar ratio of 1: 0.15.
Příklad 3Example 3
Postupuje sa ako v příkladu 2 s tým, rozdielom, že sa použije 3 %-ný vodný roztok hydroxidu draselného a 1,2 1 10 %-néhd hmot. vodného roztoku chlórnanu vápenatého. Xylány sa vyzrážajú v trojnásobnom objemovom množstve etylalkoholu a premyjú 85 % obj. etylalkoholom. Získá sa 16 % xylánu s obsahom 89 % hmot. xylózy a arabinózy v mólovom pomere 1: 0,2.The procedure was as in Example 2 except that a 3% aqueous potassium hydroxide solution and 1.2 L of a 10 wt. aqueous calcium hypochlorite solution. The xylanes are precipitated in three times the volume of ethyl alcohol and washed with 85% by volume. ethanol. 16% xylan with 89% wt. xylose and arabinose at a molar ratio of 1: 0.2.
Přikládáattaches
Postupuje sa ako v příkladu 1 s tým rozdielom, že sa použije 15 1 24 %-ného· hmotvodného roztoku hydroxidu draselného pri teplote 25 °C po dobu 6 h. Získá sa 26,5 % xylánu s obsahom 90, %„ xylózy a arabinózy v mólovom pomere 1: 0,2.The procedure was as in Example 1 except that 15 l of a 24% by weight aqueous potassium hydroxide solution was used at 25 ° C for 6 h. This yields 26.5% xylan containing 90% xylose and arabinose in a molar ratio of 1: 0.2.
P r i k 1 a d 5Example 1 and d 5
Postupuje sa ako v příkladu 2 s tým rozdielom, že sa použije pšeničná slama a 15 1 10 %-ného· hmot. vodného roztoku hydroxidu sodného s prídavkom 4,2 1 15 %-ného vodného roztoku chlórnanu sodného pri teplote 40 °C po dobu 2 h. Získá sa 30 % xylánu s obsahom 92 % hmot. xylózy a arabinózy v mólovom pomere 1: 0,19.The procedure was as in Example 2 except that wheat straw and 15 l of 10% by weight were used. aqueous sodium hydroxide solution with the addition of 4.2 L of a 15% aqueous sodium hypochlorite solution at 40 ° C for 2 h. 30% xylan with 92% wt. xylose and arabinose at a molar ratio of 1: 0.19.
Xylány predstavujú taký typ rastlinných polysadharidov, ktoré nachádzajú čoraz váčšiu aplikáclu v různých oblastlach spoločenskej praxe. Tieto polyméry můžu nájst uplatnenie pri výrobě paplera, v potravinárstve ako neutrálně plnidlá pri príprave nízkokalorických potravin, v chemickom priemysle ako surovina pre výrobu D-xylózy a xylitu. Ďalej sa xylány a ich deriváty uplatňujú ako farmaká, detergenty, flokulanty a podobné.Xylanes are a type of plant polysadharides that are increasingly used in various areas of social practice. These polymers can be used in papermaking, in the food industry as neutral fillers in the preparation of low-calorie foods, in the chemical industry as raw materials for the production of D-xylose and xylite. Furthermore, xylanes and derivatives thereof are used as pharmaceuticals, detergents, flocculants and the like.
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Cited By (1)
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WO2003008458A1 (en) * | 2001-07-17 | 2003-01-30 | Nederlandse Organisatie Voor Toegepast-Natuurwe Tenschappelijk Onderzoek Tno | Extraction of polysaccharides from vegetable and microbial material |
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Cited By (1)
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WO2003008458A1 (en) * | 2001-07-17 | 2003-01-30 | Nederlandse Organisatie Voor Toegepast-Natuurwe Tenschappelijk Onderzoek Tno | Extraction of polysaccharides from vegetable and microbial material |
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