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SK119098A3 - Process for oxidising starch - Google Patents

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Publication number
SK119098A3
SK119098A3 SK1190-98A SK119098A SK119098A3 SK 119098 A3 SK119098 A3 SK 119098A3 SK 119098 A SK119098 A SK 119098A SK 119098 A3 SK119098 A3 SK 119098A3
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Slovakia
Prior art keywords
carbohydrate
starch
acylated
hydrogen peroxide
viscosity
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SK1190-98A
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Slovak (sk)
Inventor
Dogan S Sivasligil
Theodoor M Slaghek
WIT Dirk DE
Kornelis F Gotlieb
Reinier J J Jansen
OVEREEM Hans VAN
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Kemira Chemicals Bv
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Publication of SK119098A3 publication Critical patent/SK119098A3/en

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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08BPOLYSACCHARIDES; DERIVATIVES THEREOF
    • C08B15/00Preparation of other cellulose derivatives or modified cellulose, e.g. complexes
    • C08B15/02Oxycellulose; Hydrocellulose; Cellulosehydrate, e.g. microcrystalline cellulose
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08BPOLYSACCHARIDES; DERIVATIVES THEREOF
    • C08B31/00Preparation of derivatives of starch
    • C08B31/18Oxidised starch

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Biochemistry (AREA)
  • Materials Engineering (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Polysaccharides And Polysaccharide Derivatives (AREA)
  • Medicinal Preparation (AREA)
  • Cosmetics (AREA)
  • Paper (AREA)

Abstract

A process for reducing the viscosity of polysaccharides such as starch by treatment with hydrogen peroxide in the presence of an acylated polysaccharide as an activator is described. The acylated polysaccharide is used in particular in an amount which is equivalent to at least 1 acyl group per 100 monosaccharide units. The hydrogen peroxide is preferably used at 2-20 wt.%, with respect to the total of polysaccharide and acylated polysaccharide.

Description

Spôsob oxidácie škrobuProcess for starch oxidation

Oblasť technikyTechnical field

Predložený vynález sa týka spôsobu zníženia viskozity polysacharidov oxidačnou degradáciou bez kovových katalyzátorov.The present invention relates to a method for reducing the viscosity of polysaccharides by oxidative degradation without metal catalysts.

Doterajší stav technikyBACKGROUND OF THE INVENTION

Škrob musí byť pred svojím použitím v priemyselnom meradle podrobený úprave, ktorá znižuje jeho viskozitu. Na tento účel je škrob všeobecne spracovaný oxidačné v alkalickom prostredí pri zvýšenej teplote (40 až 60 °C). Táto reakcia trvá 4 až 15 hodín napr. v prípade, keď ako oxidačné činidlo je použitý chlornan spolu s kyselinou sírovou alebo fosforečnou pri teplote asi 60 °C. Nevýhodou tohoto spôsobu je množstvo produkovanej soli a nadmerné odbúravanie škrobu.The starch must be subjected to a treatment which reduces its viscosity before being used on an industrial scale. For this purpose, starch is generally oxidized in an alkaline environment at elevated temperature (40 to 60 ° C). This reaction takes 4 to 15 hours e.g. in the case where hypochlorite is used together with sulfuric or phosphoric acid as the oxidizing agent at a temperature of about 60 ° C. The disadvantage of this method is the amount of salt produced and excessive starch degradation.

Podľa iného spôsobu sa používa peroxid vodíka spolu s prechodným kovom ako katalyzátorom. Avšak po urobenej operácii je ťažko eliminovať obvykle jedovatý katalyzátor, aj keď sa použijú zlúčeniny ako je EDTA. Ďalšou nevýhodou je zafarbenie produktu.In another method, hydrogen peroxide is used together with a transition metal catalyst. However, after the operation, it is difficult to eliminate the usually poisonous catalyst, even if compounds such as EDTA are used. Another disadvantage is the coloring of the product.

US-A-5,362,868 ukazuje spôsob, podľa ktorého je viskozita (hydroxyetyl) škrobu znížená oxidáciou s použitím peroxykyseliny. Ako peroxykyselina sú používané napr. kyselina peroxosírová ( H2 SO5) alebo kyselina peroctová. Kyselina peroxosírová musí byť pripravená na mieste z peroxidu vodíka a kyseliny sírovej alebo inak musí byť použitá soľ tejto kyseliny, čo má nevýhodu vytvárania príslušných solí ako vedľajších produktov. Reaktivita kyseliny peroctovej je nižšia a výsledkom sú dlhšie reakčné doby. V US-A5,362,868 je taktiež opísané, že reakcia s peroxidom vodíka vykazuje neprijateľné reakčné časy.US-A-5,362,868 shows a process according to which the viscosity of (hydroxyethyl) starch is reduced by oxidation using a peroxyacid. As peroxyacids, e.g. peroxosulphuric acid (H 2 SO 5 ) or peracetic acid. Peroxosulphuric acid must be prepared on site from hydrogen peroxide and sulfuric acid, or otherwise a salt of this acid must be used, which has the disadvantage of forming the respective salts as by-products. The reactivity of peracetic acid is lower and results in longer reaction times. It is also disclosed in US-A5,362,868 that reaction with hydrogen peroxide exhibits unacceptable reaction times.

Podľa DE-A-4035053 materiály na báze celulózy, ako napr. bavlna, môžu byť bielené ich reakciou s kyselinou peroctovou bez aktivátorov a súčasne ich vystavením pôsobeniu ultrazvuku (35 kHz).According to DE-A-4035053 cellulose-based materials such as e.g. cotton, they can be bleached by reacting them with activators without activators and simultaneously exposing them to ultrasound (35 kHz).

Podstata vynálezuSUMMARY OF THE INVENTION

Cieľom tohto vynálezu je poskytnúť spôsob na zníženie viskozity škrobu a iných polysacharidov jednoduchými prostriedkami bez toho, aby sa použili ťažké kovy a činidlá poskytujúce soli a bez organických vedľajších produktov.It is an object of the present invention to provide a method for reducing the viscosity of starch and other polysaccharides by simple means without using heavy metals and salt-providing agents and without organic by-products.

Tento cieľ sa dosahuje pomocou spôsobu, podľa ktorého je karbohydrát oxidovaný použitím peroxidu vodíka v prítomnosti acylovaného karbohydrátu ako katalyzátora.This object is achieved by a process according to which the carbohydrate is oxidized using hydrogen peroxide in the presence of an acylated carbohydrate catalyst.

Ako karbohydrát, ktorý môže byť spracovaný spôsobom podľa tohoto vynálezu, môže byť použitý hocaký, celkom alebo čiastočne, vodorozpústny polysacharid. Tieto zahŕňajú predovšetkým škrob a jeho frakcie a deriváty, ako napr. amylózu, etoxylovaný a karboxymetylovaný škrob. Okrem toho môže byť daným spôsobom podľa vynálezu zlepšená rozpustnosť derivátov celulózy a inulínu a jeho derivátov rovnako môže byť znížená ich viskozita.Any carbohydrate that can be processed by the process of the present invention can be any, wholly or partially, water-soluble polysaccharide. These include, in particular, starch and its fractions and derivatives, such as e.g. amylose, ethoxylated and carboxymethylated starch. In addition, the solubility of the cellulose and inulin derivatives and their derivatives can also be improved by the method of the invention, and their viscosity reduced.

Acylovaný karbohydrát použitý ako katalyzátor môže byť hocaký mono-, di- alebo polysacharid, ktorý je úplne alebo čiastočne acylovaný. Bolo zistené, že na zaistenie reakcie je nutné iba malé množstvo acylovaného karbohydrátu. Je postačujúce, ak na každých 100 jednotiek anhydroglukózy (alebo ahydrofruktózy) je prítomná jedna jednotka tetraacylovaného monosacharídu alebo ekvivalentné množstvo, tj. štyri monoacylované monosacharídové jednotky. Všeobecne je použitý ekvivalent 1 - 50 hm. % acylovaného karbohydrátu vzhľadom k celkovému množstvu karbohydrátu a acylovaného karbohydrátu, skôr však 2-20 hm. %. Termín „acylované“ zahŕňa alkanoylované (acetylované, propionylované, atď.), benzylované, sulfatované, fosforylované atď.The acylated carbohydrate used as the catalyst may be any mono-, di- or polysaccharide that is wholly or partially acylated. It has been found that only a small amount of acylated carbohydrate is required to effect the reaction. It is sufficient if for each 100 units of anhydroglucose (or ahydrofructose) one unit of tetraacylated monosaccharide or equivalent is present, ie. four monoacylated monosaccharide units. Generally, an equivalent of 1-50 wt. % of acylated carbohydrate relative to the total amount of carbohydrate and acylated carbohydrate, but rather 2-20 wt. %. The term "acylated" includes alkanoylated (acetylated, propionylated, etc.), benzylated, sulfated, phosphorylated, and the like.

Acylovaný karbohydrát môže byť jednoducho získaný reakciou karbohydrátu s acylačným činidlom, ako napr. acetanhydridom, s použitím štandardných metód. Niektoré acylované karbohydráty sú dostupné komerčne, ako napr. peracetylglukóza, -galaktóza a sacharóza a acetylovaný škrob majúci DS asi 2,5 %.The acylated carbohydrate can be easily obtained by reacting the carbohydrate with an acylating agent, such as e.g. acetic anhydride, using standard methods. Some acylated carbohydrates are available commercially, such as e.g. peracetylglucose, -galactose and sucrose, and acetylated starch having a DS of about 2.5%.

Výhodou používania karbohydrátu je, že oxidačná reakcia prebieha hladko a nevznikajú žiadne nežiadúce vedľajšie produkty ; acylovaný karbohydrát alebo jeho oxidačný produkt môže byť časťou spracovaného karbohydrátového produktu bez akýchkoľvek ťažkostí.The advantage of using a carbohydrate is that the oxidation reaction proceeds smoothly and no unwanted by-products are formed; the acylated carbohydrate or its oxidation product may be part of the processed carbohydrate product without any difficulty.

Množstvo peroxidu vodíka, ktoré má byť použité, je celkom závislé od žiadaného stupňa oxidácie. Množstvo 1 hm. % je všeobecne postačujúce ne dosiahnutie účinného stupňa viskozity. S výhodou je používané 1 - 40 hm. %, zvlášť potom 2 - 20 hm. % peroxidu vodíka, vzhľadom k celkovému množstvu karbohydrátu a acetylovaného karbohydrátu.The amount of hydrogen peroxide to be used is entirely dependent on the desired degree of oxidation. Quantity 1 wt. % is generally sufficient to achieve an effective degree of viscosity. Preferably, 1-40 wt. %, especially 2 - 20 wt. % hydrogen peroxide, based on the total amount of carbohydrate and acetylated carbohydrate.

Reakcia môže byť robená pri teplote miestnosti, ale radšej pri zvýšenej teplote, všeobecne od 20 do 90 0 C , najlepšie potom od 40 0 C do 60 0 C. Reakčná doba je od niekoľko minút po niekoľko hodín pri teplote, ktorá závisí od príslušného karbohydrátu a požadovaného stupňa viskozity.The reaction may be conducted at the room temperature, but rather at an elevated temperature, generally between 20 and 90 0 C, more preferably from 40 0 C to 60 0 C. The reaction time is from several minutes to several hours at a temperature which depends on the particular carbohydrate and the desired degree of viscosity.

Príklad uskutočnenia vynálezuDETAILED DESCRIPTION OF THE INVENTION

K suspenzii škrobu ( 70 g suchej hmotnosti v 130g vody : 35 hm. %) boli pridané 2 g pentaacetátu pri 50 0 C. Potom sa naraz pridá roztok 10 ml peroxidu vodíka (30 hm.%). Pomocou 1 N roztoku kyseliny chlorovodíkovej sa pH zníži na 1,4. Po uplynutí reakčnej doby v rozsahu medzi 15 minútami a 6 hodinami je reakčná zmes zneutralizovaná a oxidovaný škrob je oddelený filtráciou, premytý vodou a sušený acetónom. Viskozita suspenzie 20 g produktu v 380 ml vody je určená Brabendorovým viskozimetrom.To a suspension of starch (70 g dry weight in 130 g water: 35 wt%) was added 2 g pentaacetate at 50 ° C. Then a solution of 10 ml hydrogen peroxide (30 wt%) was added in one portion. The pH is lowered to 1.4 with 1N hydrochloric acid. After a reaction time of between 15 minutes and 6 hours, the reaction mixture is neutralized and the oxidized starch is collected by filtration, washed with water and dried with acetone. The viscosity of a suspension of 20 g of product in 380 ml of water is determined by a Brabendor viscometer.

Tabuľka 1 zhrňuje výsledky produktu po 3 hodinách a po 6 hodinách. Na porovnanie je rovnako uvedený výsledok spracovania pri použití samotného peroxidu vodíka po 3 hodinách.Table 1 summarizes the product results after 3 hours and 6 hours. For comparison, the treatment result using hydrogen peroxide alone after 3 hours is also shown.

Tabuľka 1Table 1

Viskozita škrobu po oxidáciiViscosity of starch after oxidation

Oxidačné činidlo Oxidizing agent Reakčná doba (h) Reaction time (h) Počiatočná teplota (0 C)1 Initial temperature ( 0 C) 1 Max. tepl. (°C)2 Max. temp. (° C) 2 Max. viskozita 3 Max. viscosity 3 Konečná viskozita 4 Final viscosity 4 žiadne (slepý pokus) none (blank) 61 61 80 80 3200 3200 1180 1180 H2O2 H 2 O 2 3 3 64 64 86 86 1560 1560 500 500 H2O2+ GluAc5H 2 O 2 + GluAc 5 3 3 64 64 72 72 520 520 120 120 H2 O2+ GluAc5H 2 O 2+ GluAc 5 6 6 66 66 >90 > 90 500 500 440 440

' Počiatočná teplota Brabenderovej krivky 2 Teplota maxima Brabenderovej krivky 3 Brabenderové jednotky pri maxime Brabenderovej krivky : 75 ot/min, tepl. gradient : 1,5°Brabender curve start temperature 2 Brabender curve maximum temperature 3 Brabender units at maximum Brabender curve: 75 rpm, temp. gradient: 1.5 °

C/min, t štart 40 °C , t kOnS-t 90 °C, udržiavacia doba : 30 minút: norma AVEBE 019142 4 Brabenderové jednotky v sedle Brabenderovej krivky (ako3)C / min, t start 40 ° C, t kO n S -t 90 ° C, holding time: 30 minutes: AVEBE 019142 4 Brabender units in the saddle of the Brabender curve (as 3 )

Claims (4)

1. Spôsob zníženia viskozity karbohydrátov reakciou s peroxidom vodíka za prítomnosti katalyzátora, vyznačujúci sa použitím acylovaného karbohydrátu ako katalyzátora.A process for reducing the viscosity of carbohydrates by reaction with hydrogen peroxide in the presence of a catalyst, characterized by the use of an acylated carbohydrate catalyst. 2. Spôsob podľa nároku 1, v ktorom je použité ekvivalentné množstvo 1 až 50 hm.% acylovaného karbohydrátu vzhľadom k celkovému množstvu karbohydrátu a acylovaného karbohydrátu.The method of claim 1, wherein an equivalent amount of 1 to 50 wt% of the acylated carbohydrate relative to the total amount of the carbohydrate and the acylated carbohydrate is used. 3. Spôsob podľa nároku 1 alebo 2, v ktorom je použité 2 až 20 hm.% peroxidu vodíka vzhľadom k celkovému množstvu karbohydrátu a acylovaného karbohydrátu.The process according to claim 1 or 2, wherein 2 to 20 wt% hydrogen peroxide based on the total amount of carbohydrate and acylated carbohydrate is used. 4. Spôsob podľa hociktorého z nárokov 1 až 3, kde karbohydrátom je škrob.The process of any one of claims 1 to 3, wherein the carbohydrate is starch.
SK1190-98A 1996-02-29 1997-02-28 Process for oxidising starch SK119098A3 (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
NL1002494A NL1002494C2 (en) 1996-02-29 1996-02-29 Method for oxidizing starch.
PCT/NL1997/000098 WO1997031951A1 (en) 1996-02-29 1997-02-28 Process for oxidising starch

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EP (1) EP0883630A1 (en)
JP (1) JP2000506197A (en)
KR (1) KR19990087307A (en)
CN (1) CN1212708A (en)
AU (1) AU723782B2 (en)
BG (1) BG102731A (en)
BR (1) BR9707771A (en)
CA (1) CA2247109A1 (en)
CZ (1) CZ266998A3 (en)
EA (1) EA000896B1 (en)
HU (1) HUP9901784A3 (en)
IL (1) IL125942A0 (en)
NL (1) NL1002494C2 (en)
NZ (1) NZ331585A (en)
PL (1) PL328613A1 (en)
SK (1) SK119098A3 (en)
TR (1) TR199801653T2 (en)
WO (1) WO1997031951A1 (en)
YU (1) YU37298A (en)
ZA (1) ZA971785B (en)

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Publication number Priority date Publication date Assignee Title
NL1007085C2 (en) * 1997-09-19 1999-03-22 Inst Voor Agrotech Onderzoek Carbohydrate oxidation with hydrogen peroxide
NL1010660C2 (en) * 1998-11-26 2000-05-30 Inst Voor Agrotech Onderzoek Method for oxidizing starch.
DE19953589B4 (en) 1999-11-08 2005-05-25 Sca Hygiene Products Gmbh Polysaccharide with functional groups, process for its preparation and products made therefrom
KR100371866B1 (en) * 2000-06-24 2003-02-11 주식회사 삼양제넥스 Modified starch useful for paper surface sizing and a method thereof
DE10241040B4 (en) * 2001-09-04 2004-11-18 Heppe Gmbh Biotechnologische Systeme Und Materialien Modified polysaccharide materials and process for their manufacture
CN101177459B (en) * 2007-11-30 2010-05-19 四川大学 Oxidized starch with high carbonyl content and its preparation method
US8641863B2 (en) * 2011-09-30 2014-02-04 Weyerhaeuser Nr Company Catalytic carboxylation of cellulose fibers in a continuous process with multiple additions of catalyst, secondary oxidant and base to a moving slurry of cellulose fibers
KR101409213B1 (en) * 2012-12-20 2014-06-19 대상 주식회사 Method for decreasing sulfurous acid included in by-products of corn wet-milling
EP3205673B1 (en) * 2016-02-12 2018-05-23 Coöperatie Avebe U.A. Oxidation of starch
EP3416740B1 (en) 2016-02-19 2021-01-06 Intercontinental Great Brands LLC Processes to create multiple value streams from biomass sources
CN114751994B (en) * 2022-03-18 2023-02-17 西南林业大学 Acetylated oxidized starch and preparation method thereof, modified urea-formaldehyde resin adhesive and preparation method and application thereof

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BE443524A (en) * 1940-07-01
NL209345A (en) * 1955-07-27
EP0492000B1 (en) * 1990-12-28 1997-04-09 AUSIMONT S.p.A. Process for increasing the bleaching efficiency of an inorganic persalt
US5362868A (en) * 1993-06-18 1994-11-08 Degussa Aktiengesellshaft Thinning of granular starch

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HUP9901784A2 (en) 1999-10-28
WO1997031951A1 (en) 1997-09-04
KR19990087307A (en) 1999-12-27
AU2235497A (en) 1997-09-16
NL1002494C2 (en) 1997-09-01
IL125942A0 (en) 1999-04-11
ZA971785B (en) 1997-09-29
NZ331585A (en) 2000-03-27
AU723782B2 (en) 2000-09-07
TR199801653T2 (en) 1998-12-21
CN1212708A (en) 1999-03-31
BR9707771A (en) 2000-01-04
YU37298A (en) 1999-09-27
EA199800778A1 (en) 1999-02-25
BG102731A (en) 1999-07-30
PL328613A1 (en) 1999-02-01
EA000896B1 (en) 2000-06-26
CA2247109A1 (en) 1997-09-04
EP0883630A1 (en) 1998-12-16
HUP9901784A3 (en) 1999-11-29
CZ266998A3 (en) 1999-03-17
JP2000506197A (en) 2000-05-23

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