EP1432739A2 - Procede et dispositif pour produire des oligomeres modifies a base de polysaccharides - Google Patents

Procede et dispositif pour produire des oligomeres modifies a base de polysaccharides

Info

Publication number
EP1432739A2
EP1432739A2 EP02782694A EP02782694A EP1432739A2 EP 1432739 A2 EP1432739 A2 EP 1432739A2 EP 02782694 A EP02782694 A EP 02782694A EP 02782694 A EP02782694 A EP 02782694A EP 1432739 A2 EP1432739 A2 EP 1432739A2
Authority
EP
European Patent Office
Prior art keywords
reactor
oligomers
pressure
polysaccharides
gas
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
EP02782694A
Other languages
German (de)
English (en)
Inventor
Andreas Heppe
Suwalee Chandrkrchang
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Heppe Biotechnologische Systeme und Materialien GmbH
Original Assignee
Heppe Biotechnologische Systeme und Materialien GmbH
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Priority claimed from DE10244333A external-priority patent/DE10244333A1/de
Application filed by Heppe Biotechnologische Systeme und Materialien GmbH filed Critical Heppe Biotechnologische Systeme und Materialien GmbH
Publication of EP1432739A2 publication Critical patent/EP1432739A2/fr
Withdrawn legal-status Critical Current

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
    • C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
    • C08B37/0006—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid
    • C08B37/0024—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid beta-D-Glucans; (beta-1,3)-D-Glucans, e.g. paramylon, coriolan, sclerotan, pachyman, callose, scleroglucan, schizophyllan, laminaran, lentinan or curdlan; (beta-1,6)-D-Glucans, e.g. pustulan; (beta-1,4)-D-Glucans; (beta-1,3)(beta-1,4)-D-Glucans, e.g. lichenan; Derivatives thereof
    • C08B37/0027—2-Acetamido-2-deoxy-beta-glucans; Derivatives thereof
    • C08B37/003—Chitin, i.e. 2-acetamido-2-deoxy-(beta-1,4)-D-glucan or N-acetyl-beta-1,4-D-glucosamine; Chitosan, i.e. deacetylated product of chitin or (beta-1,4)-D-glucosamine; Derivatives thereof

Definitions

  • the invention relates to a method for producing oligomers based on polysaccharides, consisting of particles of a few nanometers.
  • the oligomers have a low molecular weight scatter and have the property that they are not recognized as a foreign substance by plant, animal and human cells.
  • the process according to the invention shows how the modified oligomers are produced by chemical and physical process steps. Furthermore, a device for producing the oligomers and thus for implementing the method is presented.
  • oligomers are made from polysaccharides by separating the oxygen bridge between the glucose units. This separation is usually carried out with acid / alkali combinations or with hydrogen peroxide. The acid or hydrogen peroxide not only attacks the oxygen bridge, but also destabilizes the monosaccharide ring or the amino groups located on it, e.g. B. polyglucose amine. The quality, especially the cationicity of the monosaccharides or the oligomer chain is adversely affected.
  • Aqueous acidic polymer solutions are usually used as the starting material for the production of oligomers.
  • liquids with a high polymer content which are highly viscous long reaction times occur when acid or hydrogen peroxide is used, or in the case of a shorter reaction time there are high inhomogeneities in the liquid, ie. H. very scattering molecular weight distribution. It is therefore difficult to produce oligomers from suspensions with a polymer content of more than 2%.
  • Polymer contents of more than 5% are gel-like, but have the advantage that they dry quickly and form dense layers.
  • ozone is e.g. B. known in water supply and wastewater treatment.
  • the ozone causes damage to the cell walls of bacteria and viruses.
  • high-pressure dispersers or nozzles in which high shear forces arise as a result of high pressure and are used for emulsifying wax, oil and latex solutions, are also known.
  • the object of the invention is to find a gentle way that separates the polysaccharides at the oxygen bridges without reactively influencing the amino groups.
  • oligomers with a particle size of a few nanometers are to be produced.
  • the aim is to ensure that the finely dispersed particles are retained as particles and do not grow together to form associations or become liquids again.
  • the particles should be easy to separate from the air and have a large charge-active surface.
  • the oligomers should have the properties of monosaccharides that are no longer recognized as foreign substances by plant, animal and human cells.
  • an oxidizing agent e.g. B. Ozone supports the separation and secures the break point and ensures that the short chains of polysaccharide rings do not react again with each other.
  • the reaction can be controlled by pressure, temperature, shear forces, time and ozone concentration, so that modified oligomers with low molecular weight scattering are produced.
  • These short chains of polysaccharide rings with attached amino groups are produced without chemical modification of the monosaccharide groups and the amino groups present, whereby their stability is ensured.
  • a gas / suspension mixture which has large reactive surfaces and is subsequently atomized with the aid of a nozzle and high pressure is obtained from a highly viscous polymer suspension by mixing in a gas which can be reactive. The occurring The polymer chains are shared by shear forces. Then the oligomer particles get into a room, one could also say relaxation room, for further treatment.
  • the conditions in the relaxation room can be designed so that these particles dry immediately due to the small thickness and the large surface area.
  • the oligomers based on chitosan z. B. are cationically charged and would settle on anionically charged surfaces.
  • the surfaces of the relaxation room are charged cationically to prevent them from settling or accumulating.
  • An anionically charged discharge element is arranged at the outlet of the particles from the expansion space and separates the particles by changing the charge.
  • the modified oligomer particles so produced, i.e. short polysaccharide rings with attached amino groups can be placed in a storage container.
  • the present process combines in a new way several process steps in order to obtain oligomer particles as a result which are present in solid form in the size of a few nanometers or micrometers.
  • the process is easy to control; the entire process is encapsulated and can be carried out hygienically clean or carried out in a defined, temperature-controlled gas atmosphere.
  • the modified oligomers can be produced in a defined size as required.
  • the oligomers produced in this way have the properties of monosaccharides, are no longer recognized by cells as a foreign substance and can therefore get into the cell structure. Due to the cationic charges, the oligomers can attach to appropriate materials, for example to films during surface coating, or other particles can attach to the oligomers.
  • a plant which consists of two reactors.
  • a reactor known per se for. B. according to DE 43 37 625 C2
  • essentially the polysaccharides are separated into short chains and the addition of ozone in order to secure the breaking points.
  • a second reactor is used for drying and is designed in such a way that these modified particles can be removed.
  • FIG. 1 shows the plant for the production of the modified oligomers.
  • a polymer solution is introduced via a feed line 3. This supply takes place via a controllable pump 4, which receives the information about the viscosity from a measuring element 5.
  • a Pump 6 requests a continuous amount of the mixture of substances to the measuring element 5.
  • a 3-way valve 8 is arranged in the course of the pipeline 7, which, when the viscosity measuring device 5 emits a desired signal, discharges a small partial flow into a subsequent drying device or into a buffer 9 ,
  • the double control of the process is carried out with the aid of the measuring device 10 for the dissolved oxygen and measuring device 11 for the ozone content and with the aid of a pressure measuring device 12 which indicates an overpressure.
  • An adjustable gas distribution device 13 carries the fresh ozone from the ozone generator 17, into which oxygen or air is introduced via a suction opening 18, into the interior of the loop tube 19 in such a way that the flow forces are greater than the bubble buoyancy.
  • the ventilation device 14 enters the gas mixture sucked out of the upper reactor chamber 15 into the reactor chamber via a fan 16.
  • the system is controlled via the oxygen 10 and ozone content 11 in correspondence with the measurement of the viscosity 5 when monitoring an overpressure 12.
  • the pressure inside the reactor should be equal to or greater than the outside pressure.
  • a high overpressure favors a quick and fine crystalline drying in the subsequent process.
  • the polymer / ozone mixture produced is introduced into a nozzle 22 which is as oscillating as possible via a high-pressure pump 21.
  • evaporation elements 24 accelerate the evaporation of solvents, such as. B. water.
  • solvents such as. B. water.
  • the liquid particles condense to solid or plastic particles in the upper reactor chamber 25.
  • the wall 26 of the upper reactor chamber electrostatically separated from the container wall by insulators, is charged with the same polarity to the charge carriers of the polymers / oligomers by applying a voltage using a voltage source 27.
  • a blower 28 sucks air out of the upper reactor space and blows it into ring nozzles 29 in such a way that the particles are as vertical as possible
  • a counter-polar discharge element 30 is arranged above the air collection space 32 provided with a filter surface 31, which is rotatable and can be reversed in segments.
  • the particles with opposite polarity settle in the discharge element 30 and are repelled into the container 33 after rotation and polarity reversal.
  • the process can be controlled via the pressure and the geometry in the nozzle 22, the temperature and composition of the polymer mixture, the heating temperature of the evaporation elements 24 and the circulation quantity of the fan 28.
  • the separated particle size can be controlled via the applied voltage using the voltage source 27.
  • the resulting particles have a size of a few nanometers, adjustable down to the micrometer range. Further conglomerate formation of the particles is prevented if the amount of polymer injection is so small that it does not exceed the discharge capacity.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Biochemistry (AREA)
  • Molecular Biology (AREA)
  • Engineering & Computer Science (AREA)
  • General Health & Medical Sciences (AREA)
  • Materials Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Processes Of Treating Macromolecular Substances (AREA)
  • Polysaccharides And Polysaccharide Derivatives (AREA)

Abstract

L'invention concerne un procédé et un dispositif pour produire des oligomères modifiés à base de polysaccharides comportant des groupes amino fixés par addition. Constitués de particules de quelques nanomètres, ces oligomères ont une faible dispersion de masse molaire et la propriété de ne pas être identifiés comme corps étranger par les cellules végétales, animales et humaines. L'invention concerne un procédé pour séparer avec précaution les polysaccharides au niveau des ponts oxygène, sans influencer de manière réactive les groupes amino. On a constaté de façon surprenante que les forces de liaison électrophysiques des ponts oxygène supportent moins les sollicitations mécaniques que les composés cycliques et qu'elles rompent sous l'effet de certaines forces de cisaillement. La réaction est conduite dans des contenants en faisant intervenir les facteurs pression, température, forces de cisaillement, temps et concentration d'ozone. Les polysaccharides séchés comportant des groupes amino fixés par addition sont chargés cationiquement. Les oligomères se fixent sur un élément d'évacuation de pôle opposé et ils sont rejetés pour prélèvement par inversion de polarité.
EP02782694A 2001-09-27 2002-09-25 Procede et dispositif pour produire des oligomeres modifies a base de polysaccharides Withdrawn EP1432739A2 (fr)

Applications Claiming Priority (5)

Application Number Priority Date Filing Date Title
DE10148694 2001-09-27
DE10148694 2001-09-27
DE10244333A DE10244333A1 (de) 2001-09-27 2002-09-19 Verfahren und Einrichtung zur Herstellung von modifizierten Oligomeren auf der Basis von Polysacchariden
DE10244333 2002-09-19
PCT/DE2002/003675 WO2003029297A2 (fr) 2001-09-27 2002-09-25 Procede et dispositif pour produire des oligomeres modifies a base de polysaccharides

Publications (1)

Publication Number Publication Date
EP1432739A2 true EP1432739A2 (fr) 2004-06-30

Family

ID=26010280

Family Applications (1)

Application Number Title Priority Date Filing Date
EP02782694A Withdrawn EP1432739A2 (fr) 2001-09-27 2002-09-25 Procede et dispositif pour produire des oligomeres modifies a base de polysaccharides

Country Status (4)

Country Link
EP (1) EP1432739A2 (fr)
CA (1) CA2461906A1 (fr)
NO (1) NO20041940L (fr)
WO (1) WO2003029297A2 (fr)

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB201912061D0 (en) 2019-08-22 2019-10-09 Biocyto Ltd Composition

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5984938A (ja) * 1982-11-04 1984-05-16 Daicel Chem Ind Ltd キトサン懸濁液およびその製造方法
JPS624703A (ja) * 1985-07-02 1987-01-10 Tooa Eiyoo Kk 低分子量へパリン画分の製法
FR2701030B1 (fr) * 1993-01-20 1995-04-07 Aber Technologies Procédé pour l'hydrolyse de chitine et/ou de chitosane et oligomères de chlorhydrate de D-glucosamine obtenus.
WO1998042718A1 (fr) * 1997-03-26 1998-10-01 The Brigham And Women's Hospital, Inc. Procede de production de fragments de saccharide

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
None *
See also references of WO03029297A3 *

Also Published As

Publication number Publication date
WO2003029297A2 (fr) 2003-04-10
NO20041940L (no) 2004-04-26
CA2461906A1 (fr) 2003-04-10
WO2003029297A3 (fr) 2003-05-22

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