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WO2000073350A2 - Procede de production d'ethers d'amidon hydroxyalkyle en poudre a utiliser comme adjuvant de pulverisation - Google Patents

Procede de production d'ethers d'amidon hydroxyalkyle en poudre a utiliser comme adjuvant de pulverisation Download PDF

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Publication number
WO2000073350A2
WO2000073350A2 PCT/DE2000/001518 DE0001518W WO0073350A2 WO 2000073350 A2 WO2000073350 A2 WO 2000073350A2 DE 0001518 W DE0001518 W DE 0001518W WO 0073350 A2 WO0073350 A2 WO 0073350A2
Authority
WO
WIPO (PCT)
Prior art keywords
starch
preparation
oxide
reaction
hydroxyalkyl
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.)
Ceased
Application number
PCT/DE2000/001518
Other languages
German (de)
English (en)
Other versions
WO2000073350A3 (fr
Inventor
Michael Meerbote
Holger Mosinski
Ursula Decker
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.)
Dow Olefinverbund GmbH
Original Assignee
Buna Sow Leuna Olefinverbund 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
Application filed by Buna Sow Leuna Olefinverbund GmbH filed Critical Buna Sow Leuna Olefinverbund GmbH
Publication of WO2000073350A2 publication Critical patent/WO2000073350A2/fr
Anticipated expiration legal-status Critical
Publication of WO2000073350A3 publication Critical patent/WO2000073350A3/fr
Ceased legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
    • C08B31/00—Preparation of derivatives of starch
    • C08B31/08—Ethers
    • C08B31/12—Ethers having alkyl or cycloalkyl radicals substituted by heteroatoms, e.g. hydroxyalkyl or carboxyalkyl starch

Definitions

  • the products produced according to the invention are particularly suitable for applications as spray aids, also in combination with other customary spray aid additives, in the processing of aqueous polymer dispersions, prepared on the basis of various vinyl esters, their mixtures and combinations with other monomers, in particular with alkanes.
  • the propoxylation can be carried out in a 40-45% aqueous alkaline suspension (for example US Pat. No. 1,876,920, US Pat. No. 2,516,634, US Pat. No. 3,033,853).
  • sodium sulfate or sodium chloride US Pat. No. 2,516,634, US Pat. No. 3,378,546, US Pat. No. 3,422,088, US Pat. No. 3,577,407, EP 0 313 298
  • DE 2 109 015 worked with a separate upstream catalytic activation of the starch in the presence of sodium chloride.
  • the alkoxylations in aqueous systems are carried out at temperatures between 40-80 ° C. In any case, below the gelatinization temperature must be implemented if filterable products are to be obtained.
  • the reaction times of such process variants depend on the desired one Degree of alkoxylation and can be up to 40 hours. For products with extraordinarily low degrees of substitution, they average 8-12 hours.
  • Variants of this process use aqueous solutions of short-chain alcohols, such as, for example, methanol (JP 57 030 701) or ethanol (EP 0 109 776).
  • the alcohols mentioned can also serve as solvents in undiluted form (US Pat. No. 2,845,417) or other alcohols, such as, for example, isopropanol (US Pat. No.
  • protective colloid especially for the spray drying process of 'polymer dispersions, depends on the different development goals, e.g. B. the viscosity and flow behavior of a dispersion, the field of use of the dispersions or the polymer powder, influencing the spray drying process in the production of redispersible powder, the redispersion behavior of the polymer powder, u. a.
  • the cyclone yield and the associated tower covering are important parameters when assessing a spray drying process.
  • This object is achieved in that the starch is reacted in a mixture of an excess of C 3 / C 4 alkylene oxide and an optimal amount of ethylene oxide in the presence of an alkaline catalyst.
  • the response times are usually more than 15 hours.
  • the products obtained are moreover characterized by a surprisingly low oligoalkylene glycol content of less than 2% by weight, based on the starch used.
  • hydroxyalkyl starch ethers produced according to the invention are outstandingly suitable as spraying aids in the working up of aqueous polymer dispersions. Their use is problem-free and leads to no caking phenomena during the process on the tower wall.
  • hydroxyalkyl starch ethers produced according to the invention are suitable simultaneously in all known applications in construction chemistry and as a protective colloid in the known emulsion polymerization processes.
  • reaction is terminated by vigorous cooling and / or neutralization using known organic or inorganic acids, the reaction product is separated off using conventional workup methods and the remaining, unreacted propylene oxide is recovered.
  • analysis and characterization of the reaction product was carried out by means of gel permeation chromatography (GPC), H 1 -NMR spectroscopy as well as the Ninhydri ⁇ method to determine the degree of substitution of the modified starch.
  • the unreacted alkylene oxide portion was analyzed using headspace gas chromatography.
  • Example 2 (modified comparative example):
  • 162 g of corn starch (moisture content 12.3%) are placed in a pressure autoclave apparatus corresponding to the prior art.
  • the apparatus is flushed several times with nitrogen and subsequently charged with 600 g of propylene oxide, 3.24 g of NaOH in the form of a 50% strength aqueous solution, and a nitrogen pressure of 0.5 bar is set.
  • the reaction mixture is then heated to a temperature of 70 ° C. with constant stirring and kept at this temperature for 6 hours. This creates a pressure of 3.0 to 4.0 bar.
  • the reaction product was worked up and characterized analogously to Example 1.
  • HEPS hydroxyethyl propyl starch

Landscapes

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

Abstract

L'invention concerne un procédé de production d'éthers d'amidon hydroxyalkylé présentant un indice d'hydroxyle compris entre 350 et 600 et un degré de substitution molaire de 1 à 2. Lesdits éthers sont obtenus par alcoxylation d'hydrates de carbone alcalinisés avec un mélange d'oxydes de propylène-d'éthylène. Les produits obtenus selon ledit procédé conviennent particulièrement pour une utilisation en tant qu'adjuvant de pulvérisation. Le procédé décrit est mis en oeuvre en présence de catalyseurs, de préférence alcalins. La quantité totale d'un oxyde d'alkylène C3-C4, de préférence d'oxyde de propylène, requise pour la réaction avec l'amidon est mise à réagir avec 10 à 60 % en poids d'oxyde d'éthylène, par rapport à la quantité totale d'oxyde d'alkylène, à des températures pouvant aller de 40 °C à 80 °C.
PCT/DE2000/001518 1999-05-29 2000-05-13 Procede de production d'ethers d'amidon hydroxyalkyle en poudre a utiliser comme adjuvant de pulverisation Ceased WO2000073350A2 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE19924773.0 1999-05-29
DE1999124773 DE19924773A1 (de) 1999-05-29 1999-05-29 Verfahren zur Herstellung pulverförmiger Hydroxyalkylstärkeether für den Einsatz als Sprühhilfsmittel

Publications (2)

Publication Number Publication Date
WO2000073350A2 true WO2000073350A2 (fr) 2000-12-07
WO2000073350A3 WO2000073350A3 (fr) 2002-10-03

Family

ID=7909674

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/DE2000/001518 Ceased WO2000073350A2 (fr) 1999-05-29 2000-05-13 Procede de production d'ethers d'amidon hydroxyalkyle en poudre a utiliser comme adjuvant de pulverisation

Country Status (2)

Country Link
DE (1) DE19924773A1 (fr)
WO (1) WO2000073350A2 (fr)

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE1019288B (de) * 1953-05-19 1957-11-14 Union Carbide Corp Verfahren zur Herstellung von fester, granulierter, wasserloeslicher Oxyalkylstaerke
US4585858A (en) * 1967-01-03 1986-04-29 Cpc International Inc. Starch-based polyether polyols
US3903076A (en) * 1974-06-26 1975-09-02 Dow Chemical Co Preparation and purification of cellulose ethers
DE3919729C3 (de) * 1989-06-16 1997-06-19 Fresenius Ag Hydroxyethylstärke als Plasmaexpander, Verfahren zu ihrer Herstellung und Verwendung als kolloidales Plasmaersatzmittel

Also Published As

Publication number Publication date
DE19924773A1 (de) 2000-11-30
WO2000073350A3 (fr) 2002-10-03

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