SE406330B - STORAGE STABLE POLYVINYLESTER-BASED ONE-COMPONENT ADHESIVE CONTAINING POLYVINYL ALCOHOL AS A PROTECTIVE COLOID AND AN URBAN FORMALDEHYDE ADDUCT AND AN ACID METAL SALT - Google Patents

STORAGE STABLE POLYVINYLESTER-BASED ONE-COMPONENT ADHESIVE CONTAINING POLYVINYL ALCOHOL AS A PROTECTIVE COLOID AND AN URBAN FORMALDEHYDE ADDUCT AND AN ACID METAL SALT

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SE406330B
SE406330B SE7316881A SE7316881A SE406330B SE 406330 B SE406330 B SE 406330B SE 7316881 A SE7316881 A SE 7316881A SE 7316881 A SE7316881 A SE 7316881A SE 406330 B SE406330 B SE 406330B
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weight
water
polyvinyl alcohol
metal salt
dispersion
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SE7316881A
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Swedish (sv)
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J Eb
R Muller
A Homanner
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Hoechst Ag
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Priority claimed from DE19722261402 external-priority patent/DE2261402C3/en
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Publication of SE406330B publication Critical patent/SE406330B/en

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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J131/00Adhesives based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an acyloxy radical of a saturated carboxylic acid, of carbonic acid, or of a haloformic acid; Adhesives based on derivatives of such polymers
    • C09J131/02Homopolymers or copolymers of esters of monocarboxylic acids
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/16Halogen-containing compounds
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/24Acids; Salts thereof
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/28Nitrogen-containing compounds
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/30Sulfur-, selenium- or tellurium-containing compounds
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L29/00Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal or ketal radical; Compositions of hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Compositions of derivatives of such polymers
    • C08L29/02Homopolymers or copolymers of unsaturated alcohols
    • C08L29/04Polyvinyl alcohol; Partially hydrolysed homopolymers or copolymers of esters of unsaturated alcohols with saturated carboxylic acids
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L31/00Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an acyloxy radical of a saturated carboxylic acid, of carbonic acid or of a haloformic acid; Compositions of derivatives of such polymers
    • C08L31/02Homopolymers or copolymers of esters of monocarboxylic acids
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2666/00Composition of polymers characterized by a further compound in the blend, being organic macromolecular compounds, natural resins, waxes or and bituminous materials, non-macromolecular organic substances, inorganic substances or characterized by their function in the composition
    • C08L2666/02Organic macromolecular compounds, natural resins, waxes or and bituminous materials
    • C08L2666/14Macromolecular compounds according to C08L59/00 - C08L87/00; Derivatives thereof
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2666/00Composition of polymers characterized by a further compound in the blend, being organic macromolecular compounds, natural resins, waxes or and bituminous materials, non-macromolecular organic substances, inorganic substances or characterized by their function in the composition
    • C08L2666/54Inorganic substances
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L61/00Compositions of condensation polymers of aldehydes or ketones; Compositions of derivatives of such polymers
    • C08L61/20Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen
    • C08L61/22Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes with acyclic or carbocyclic compounds
    • C08L61/24Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes with acyclic or carbocyclic compounds with urea or thiourea

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Adhesives Or Adhesive Processes (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Description

7316881 1-7 Man har nu funnit ett enkomponentlim på basis av en vatten- haltig polyvinylalkohol som skyddskolloid innehållande polyvinyl- esterdispersion, som har en förhöjd vattenbeständighet och god lag- ringsstabilitet, när det innehåller 1 - 15 vikts-% polyvinylalkohol, angivet på dispersionens polymerisatandel, 1,5 till 3 vikts-% av en vattenlöslig karbamid-formaldehyd-addukt, som i huvudsak består av mono- till tetrametylolkarbamid, och 0,05 till 0,5 vikts-% av ett vattenlösligt, surt metallsalt. 7316881 1-7 A one-component adhesive has now been found on the basis of an aqueous polyvinyl alcohol as a protective colloid containing polyvinyl ester dispersion, which has an increased water resistance and good storage stability, when it contains 1 - 15% by weight of polyvinyl alcohol, indicated on the dispersion. polymer component, 1.5 to 3% by weight of a water-soluble urea-formaldehyde adduct, consisting essentially of mono- to tetramethylol urea, and 0.05 to 0.5% by weight of a water-soluble acidic metal salt.

Som vattenhaltiga polyvinylesterdispersioner är polymerisat- lgdispersioner av homo- eller sampolymerisat av vinylestrar sinsemel- lan eller med ytterligare, etyleniskt omättade monomerer lämpade, varvid andelen inpolymeriserad vinylester i polymerisatet uppgår till åtminstone 50 vikts-%. Som vinylestrar används vinylestrarna av mättade, alifatiska monokarbonsyror med 1 - 18 C-atomer, t.ex. vinylformiat, vinylacetat, vinylpropionat, vinylisobutyrat, vinyl- laurat, vinylestrar av mättade, grenade monokarbonsyror med 9 - 11 C-atomer eller vinylstearat, företrädesvis vinylacetat. Ytterligare etyleniskt omättade monomerer, som kan sampolymeriseras med vinyl- estrarna, är akryl- eller metakrylsyra eller estrar av dessa med mättade, envärda, alifatiska alkoholer med 1 - 8 C-atomer, mono- eller diestrar av a,ß-etyleniskt omättade dikarbonsyror såsom ma- lein-, fumar-, itakon- eller citrakonsyra med mättade, envärda, alifatiska alkoholer med 1 - 8 C-atomer, etyleniskt omättade kol- väten, t.ex. eten, a-olefiner med 3 - 12 C-atomer, styren, vinyl- toluen eller vinylxylen, halogenerade, omättade, alifatiska kolväen, t.ex. vinylklorid, vinylflourid, vinylidenklorid eller vinyliden- fluorid, samt kvävehaltiga derivat av akryl- eller metakrylsyra, t.ex. akrylnitril, akrylamid eller N-metylolakrylamid. De vatten- haltiga polyvinylesterdispersionerna kan eventuellt även innehålla upp till 10 viktsprocent, angivet på den totala mängden av alla monomerer, förnätande.monomerer med åtminstone två etyleniska dub- belbindningar i molekylen inpolymeriserade i polymerisatet, t.ex. diallylftalat, diallylmaleinat, triallylcyanurat, tetraallyloxietan divinylbensen, butandiol-1,h-dimetakrylat eller trietyënglykoldi- metakrylat.Suitable aqueous polyvinyl ester dispersions are polymeric layer dispersions of homo- or copolymers of vinyl esters with each other or with additional ethylenically unsaturated monomers, the proportion of polymerized vinyl ester in the polymer being at least 50% by weight. The vinyl esters used are the vinyl esters of saturated aliphatic monocarboxylic acids having 1 to 18 carbon atoms, e.g. vinyl formate, vinyl acetate, vinyl propionate, vinyl isobutyrate, vinyl laurate, vinyl esters of saturated, branched monocarboxylic acids having 9 to 11 carbon atoms or vinyl stearate, preferably vinyl acetate. Additional ethylenically unsaturated monomers which can be copolymerized with the vinyl esters are acrylic or methacrylic acid or esters thereof with saturated monohydric aliphatic alcohols having 1 to 8 carbon atoms, mono- or diesters of α, β-ethylenically unsaturated dicarboxylic acids such as maleic, fumaric, itaconic or citraconic acid with saturated monohydric aliphatic alcohols having 1 to 8 carbon atoms, ethylenically unsaturated hydrocarbons, e.g. ethylene, α-olefins having 3 to 12 carbon atoms, styrene, vinyl toluene or vinyl xylene, halogenated, unsaturated, aliphatic hydrocarbons, e.g. vinyl chloride, vinyl fluoride, vinylidene chloride or vinylidene fluoride, and nitrogen-containing derivatives of acrylic or methacrylic acid, e.g. acrylonitrile, acrylamide or N-methylolacrylamide. The aqueous polyvinyl ester dispersions may optionally also contain up to 10% by weight, indicated on the total amount of all monomers, crosslinking monomers having at least two ethylenic double bonds in the molecule polymerized in the polymer, e.g. diallyl phthalate, diallyl maleinate, triallyl cyanurate, tetraallyloxyethane divinylbenzene, butanediol-1, h-dimethacrylate or triethylene glycol dimethacrylate.

De vattenhaltiga polyvinylesterdispersionerna innehåller vi- dare som skyddskolloid 1 - 15 vikts-%, företrädesvis 4 - 12 vikts-%, angivet på polymerisatet, polyvinylalkohol, som kan tillsättes före, under eller efter polymerisationen. För att uppnå vissa användnings- 1316881-7' 3 tekniska egenskaper hos limmet såsom öppen tid, bindningstid, bind- styrka och temperaturbeständighet är det ofta fördelaktigt att an~ vända blandningar av olika vattenhaltiga polyvinylesterdispersioner.The aqueous polyvinyl ester dispersions further contain as protective colloid 1 to 15% by weight, preferably 4 to 12% by weight, indicated on the polymer, polyvinyl alcohol, which can be added before, during or after the polymerization. In order to achieve certain application properties of the adhesive such as open time, bonding time, bond strength and temperature resistance, it is often advantageous to use mixtures of different aqueous polyvinyl ester dispersions.

Företrädesvis används vattenhaltiga polyvinylaoetatdispersioner, speciellt homopolymera polyvinylacetatdispersioner. Halten fast substans hos de vattenhaltiga polyvinylesterdispersionerna uppgår till omkring #0 - 60 vikts-%.Preferably aqueous polyvinyl acetate dispersions are used, especially homopolymeric polyvinyl acetate dispersions. The solids content of the aqueous polyvinyl ester dispersions is about # 0 - 60% by weight.

Framställningen av de vattenhaltiga polyvinylesterdispersio- nerna sker på känt sätt genom radikalisk polymerisation av monome- rerna i vattenhaltig dispersion och söks ej skyddad här.The preparation of the aqueous polyvinyl ester dispersions takes place in a known manner by radical polymerization of the monomers in aqueous dispersion and is not sought to be protected here.

De vattenlösliga, lågkondenserade karbamid-formaldehydhart- :ærna erhålles genom kondensation av karbamid och formaldehyd i molförhållandet 1:1 till 1:4, företrädesvis 1:2 till 1:5, och före- ligger i form av en vattenhaltig lösning med #0 till 70 vikts-% hartshalt. Lösningarna innehåller övervägande de enkla metylol- karbamidföreningarna mono-, di-, tri- och tetrametylolkarbamid.The water-soluble, low-condensed urea-formaldehyde resins are obtained by condensation of urea and formaldehyde in the molar ratio 1: 1 to 1: 4, preferably 1: 2 to 1: 5, and are in the form of an aqueous solution with # 0 to 70% by weight resin content. The solutions predominantly contain the simple methylol urea compounds mono-, di-, tri- and tetramethylol urea.

Limmet enligt uppfinningen innehåller omkring 1,5 till 3 vikts-%, angivet på den totala blandningen, av den vattenhaltiga lösningen av det lågkondenserade karbamid-formaldehydhartset.The adhesive according to the invention contains about 1.5 to 3% by weight, indicated on the total mixture, of the aqueous solution of the low-condensed urea-formaldehyde resin.

Som vattenlösliga, sura metallsalter används sådana metall- salter som reagerar med polyvinylalkohol under förnätning, exempel- vis salter av aluminium, järn, krom, titan, zirkonium eller vanadin.As water-soluble, acidic metal salts, such metal salts which react with polyvinyl alcohol during crosslinking are used, for example salts of aluminum, iron, chromium, titanium, zirconium or vanadium.

Lämpliga salter är aluminiumnitrat, järn(III)-klorid, krom(III)- -nitrat, titanylsulfat, zirkonoxiklorid eller vanadylsulfat, företrä- desvis aluminiumklorid. Tillsatsmängderna uppgår till 0,05 till 0,3 vikts-% (fast) respektive 0,5 till 3 vikts-%, angivet på den to- tala blandningen, av en 10-procentig vattenlösning.Suitable salts are aluminum nitrate, ferric chloride, chromium (III) nitrate, titanyl sulphate, zirconium chloride or vanadyl sulphate, preferably aluminum chloride. The addition amounts amount to 0.05 to 0.3% by weight (solid) and 0.5 to 3% by weight, respectively, indicated on the total mixture, of a 10% aqueous solution.

Vidare kan för förbättring av limmets filmbildning vid rums- temperatur tillsättas kända filmbildningshjälpmedel, t.eX. glykol- syrabutylester eller butyldiglykolacetat, i mängder av omkring 1 till 3 vikts-%, angivet på den totala blandningen.Furthermore, to improve the film formation of the adhesive at room temperature, known film-forming aids can be added, e.g. glycolic acid butyl ester or butyl diglycol acetate, in amounts of about 1 to 3% by weight, indicated on the total mixture.

Enkomponentlimmet enligt uppfinningen ger trä- och pappers- hoplimningar, som kan utsättas för längre fuktrums- och kallvattens- lagringar utan att limningen löses, för vilket tidigare vattenhal-_ tiga polyvinylesterdispersioner inte var lämpade eller endast var lämpade som tvåkomponentsystem. Lagringsbeständigheten uppgår till åtminstone ett år utan att limmet förlorar sin anväñdningsförmåga och motsvarar därmed lagringsbeständigheten hos de kända dispersions- limmen. Även de övriga fördelaktiga egenskaperna hos goda dispersions- . :w ...|............. i . . 7316661-7 A tlim såsom lång öppen tid, kort bindningstid, hög bindhållfasthet och god temperaturbeständighet hos limfbgen bibehålles. Limmet _ enligt uppfinningen lämpar sig vidare för hoplimning av presskikts- lämnen, skumämnen, textilier, läder, asbestcement och andra porösa material.The one-component adhesive according to the invention provides wood and paper adhesives which can be subjected to longer humidity and cold water storage without the adhesive being dissolved, for which previously aqueous polyvinyl ester dispersions were not suitable or were only suitable as two-component systems. The shelf life is at least one year without the adhesive losing its usability and thus corresponds to the shelf life of the known dispersion adhesives. Also the other beneficial properties of good dispersion. : w ... | ............. i. . 7316661-7 Adhesives such as long open time, short bonding time, high bond strength and good temperature resistance of the adhesive are maintained. The adhesive according to the invention is further suitable for gluing together press layer residues, foam blanks, textiles, leather, asbestos cement and other porous materials.

I nedanstående exempel belyses uppfinningen närmare: Exempel 1 »Ett lim med följande sammansättning framställdes: 95, 5 viktsaéiar av en So-procentig, vattennaitig, hemo- polymer polyvinylacetatdispersion med 7 % polyvinyl- alkohol som skyddskolloid, 1,5 viktsdelar av en 50-procentig, vattenhaltig lösning av ett lågkondenserat karbamid-formaldehydharts, 1,5 viktsdelar av en 10-procentig, vattenhaltig lösning av aluminiumklorid, 5 1,5 viktsdelar glykolsyrabutylester.The following examples illustrate the invention in more detail: Example 1 An adhesive with the following composition was prepared: 95.5% by weight of a 5%, aqueous, hemopolymeric polyvinyl acetate dispersion with 7% polyvinyl alcohol as protective colloid, 1.5 parts by weight of a 50% percent aqueous solution of a low condensed urea-formaldehyde resin, 1.5 parts by weight of a 10% aqueous solution of aluminum chloride, 1.5 parts by weight of glycolic acid butyl ester.

En torkad film av detta lim vitnar inte efter längre vatten- lagring och reemulgerar inte heller medan filmer från kända dis- persionslim sväller kraftigt eller är fullständigt reemulgerbara.A dried film of this adhesive does not whiten after longer water storage and does not re-emulsify, while films from known dispersion adhesives swell sharply or are completely re-emulsifiable.

Exempel 2 Ett lim av 38,0 viktsdelar av en 50-procentig, vattenhaltig homo- polymer polyvinylacetatdispersion med 10 % polyvinyl- ' alkohol som skyddskolloid, üfl 37,5 viktsdelar av en 50-procentig, vattenhaltig homo- polymer polyvinylacetatdispersion med 5 % polyvinyl- alkohol som skyddskolloid, - 1,5 viktsdelar av en 50-procentig, vattenhaltig lösning- ' av ett lågkondenserat karbamid-formaldehydharts, 1,5 viktsdelar av en 10-procentig, vattenhaltig lösning av aluminiumnitrat och 1,5 viktsdelar glykolsyra- butylester göts till en film. Som jämförelse behandlades en känd vattenhal-' tig, homopolymer polyvinylacetatdispersion med 50 viktsprocent fast- substanshalt och 5 % polyvinylalkohol som skyddskolloid på samma sätt. Före filmframställningen sätts något vatten till limmet enligt uppfinningen och jämförelsedispersionen för att avlägsna luftblåsorna. Genom uppgjutning av en avvägd mängd på en jämn, 7316881 -7 -s med en omgivande kant försedd polyetenplatta erhålls filmer med en torrfilmtjocklek av 0,8 mm, som klimatiseras 7 dagar vid 2300 och 50 % relativ luftfuktighet.Example 2 An adhesive of 38.0 parts by weight of a 50% aqueous homopolymeric polyvinyl acetate dispersion with 10% polyvinyl alcohol as a protective colloid, ü fl 37.5 parts by weight of a 50% aqueous homopolymeric polyvinyl acetate dispersion with 5% polyvinyl alcohol as protective colloid, - 1.5 parts by weight of a 50% aqueous solution of a low condensed urea-formaldehyde resin, 1.5 parts by weight of a 10% aqueous solution of aluminum nitrate and 1.5 parts by weight of glycolic acid butyl ester were cast to a movie. For comparison, a known aqueous, homopolymeric polyvinyl acetate dispersion having a 50% strength by weight solids content and 5% polyvinyl alcohol was treated as a protective colloid in the same manner. Prior to film production, some water is added to the adhesive of the invention and the comparative dispersion to remove the air bubbles. By casting a balanced amount on a smooth, polyethylene board provided with a surrounding edge, films with a dry film thickness of 0.8 mm are obtained, which are air-conditioned for 7 days at 2300 and 50% relative humidity.

Filmernas vattenupptagning bestäms genom nedläggning i vat- ten av 2000 och efterföljande Vägning efter vattenlagring i 15, 60, 120, 240 minuter och 24 timmar. En film av limmas enligt uppfin- ningen är väsentligt mer vattenbeständig än en sådan av jämförelse- dispersionen såsom nedanstående tabell I visar: ÉâPÉll_l Vattenupptagning i % av en limfilm enligt Exempel 2 film från jämförelse; dispersionen efter 15 min 6 18 H 60 " i 10 50 H 120 H 15 32 " 240 " 15 2 inte längre mätbar " 24 tim 15 filmen sönderfaller Exempel 5 Limmet bestod av 95,0 viktsdelar av en 50-procentig, vattenhaltig, homopolymer polyvinylacetatdispersion med 7 % polyvinylalkohol som skyddskolloid, ' 3,0 viktsdelar av en 50-procentig, vattenhaltig lösning av ett lågkondenserat karbamid-formaldehydharts, 2,5 viktsdelar av en 10-procentig, vattenhaltig lösning av krom(III)-nitrat och 1,5 viktsdelar glykolsyrabutylester.The water uptake of the films is determined by immersion in water of 2000 and subsequent weighing after water storage for 15, 60, 120, 240 minutes and 24 hours. A film of adhesive according to the invention is substantially more water resistant than one of the comparative dispersion as shown in Table I below: ÉâPÉll_1 Water uptake in% of an adhesive film according to Example 2 film from comparison; the dispersion after 15 minutes 6 18 H 60 "in 10 50 H 120 H 15 32" 240 "15 2 no longer measurable" 24 hours 15 the film decomposes Example 5 The adhesive consisted of 95.0 parts by weight of a 50%, aqueous, homopolymeric polyvinyl acetate dispersion with 7% polyvinyl alcohol as protective colloid, 3.0 parts by weight of a 50% aqueous solution of a low condensed urea-formaldehyde resin, 2.5 parts by weight of a 10% aqueous solution of chromium (III) nitrate and 1.5 parts by weight parts by weight of glycolic acid butyl ester.

Med detta lim och med ett jämförelselim i form av en känd vattenhaltig homopolymer polyvinylacetatdispersion med 50 vikts-% fastsubstanshalt och 5 % polyvinylalkohol som skyddskolloid limma» des provkroppar av bokmassivträ enligt DIN 53254 och efterkontrol- lerades efter lagringsföljd 1 samt undersöktes vad avser vattenbef ständighet efter lagringsföljd 4 och 5 (DIN 53254). Lagringsföljd 1 består av en 7 dagars klimatisering av provkropparna vid 20°C och 65 % rel. luftfuktighet, lagringsföljd 4 av en 7 dagars klimatise- ring vid 20°C och 65 % relativ luftfuktighet och efterföljande 24 731688157 6 timmars vattenlagring; medan enligt lagringsföljd 5 därefter föl- jer åter en 7 dagars klimatisering vid 20°C och 65 % rel. luft- fuktighet. Bindhållfastheten efter lagringsföljd 5 betecknas äve som återtorkningshållfasthet. 1 Nedanstående tabell II åskådliggör de erhållna resultaten: Tabell II Bindnåiifasthet i kp/cmz enligt DIN 55254 för de limmade provkropparna « med ett lim med ett jämförelse- enligt Exempel 3 medel efter lagringsföljd 1 120 120 n n LI, 1 8 O " " 5 115 O Bindhållfastheten hos limningen med limmet enligt uppfin- ningen är fortfarande mätbar efter 24 timmars vattenlagring, medan provkropparna med jämförelseslimmet sönderfaller i vatten. Åter- torkningshållfastheten hos provkropparna med limmet enligt upp- finningen uppnår i det närmaste utgångsbindningshållfasthetens värde (efter lagringsföljd 1).With this glue and with a comparative glue in the form of a known aqueous homopolymer polyvinyl acetate dispersion with 50% by weight solids content and 5% polyvinyl alcohol as protective colloid, specimens of beech solid wood were glued according to DIN 53254 and checked after storage sequence 1 and examined for water. storage sequence 4 and 5 (DIN 53254). Storage sequence 1 consists of a 7-day air conditioning of the specimens at 20 ° C and 65% rel. humidity, storage sequence 4 of a 7 day air conditioning at 20 ° C and 65% relative humidity and subsequent 24 hours of water storage; while according to storage sequence 5, a 7-day air conditioning at 20 ° C and 65% rel. humidity. The bond strength after storage sequence 5 is also referred to as re-drying strength. Table II below illustrates the results obtained: Table II Bonding strength in kp / cm2 according to DIN 55254 for the glued specimens «with an adhesive with a comparison- according to Example 3 means after storage sequence 1 120 120 nn LI, 1 8 O" "5 115 The bond strength of the adhesive with the adhesive according to the invention is still measurable after 24 hours of water storage, while the test specimens with the comparative adhesive decompose in water. The re-drying strength of the test specimens with the adhesive according to the invention almost reaches the value of the starting bond strength (after storage sequence 1).

Claims (5)

1vs1saa1-7 PATENTKRAV1vs1saa1-7 PATENT REQUIREMENTS 1. Lagringsstabilt enkomponentlim på basis av en vatten- haltig polyvinylalkohol som skyddskolloid innehållande polyvinyl- esterdispersion, k ä n n e t e c k n a t a v att det innehåfler 1 - 15 viktsprocent polyvinylalkohol, angivet på dispersionens polymerisatandel, 1,5 till 3 viktsprocent av en vattenlöslig, karbamid-formaldehyd-addukt, som i huvudsak består av mono- till tetrametylolkarbamid, och 0,05 till 0,3 viktsprocent av ett vat- tenlösligt, surt metallsalt.Storage-stable one-component adhesive based on an aqueous polyvinyl alcohol as a protective colloid containing polyvinyl ester dispersion, characterized in that it contains 1 to 15% by weight of polyvinyl alcohol, indicated on the polymer fraction of the dispersion, 1.5 to 3% by weight of a water-soluble, carbamide-water-soluble adduct, which consists essentially of mono- to tetramethylol urea, and 0.05 to 0.3% by weight of a water-soluble, acidic metal salt. 2. Lim enligt krav 1, k ä n n e t e c k n a t a v att polyvinylesterdispersionerna innehåller åtminstone 50 viktspro- cent, angivet på polymerisatandelen, av inpolymeriserad vinyl- ester.Adhesives according to Claim 1, characterized in that the polyvinyl ester dispersions contain at least 50% by weight, indicated on the proportion of polymeris, of polymerized vinyl ester. 3. Lim enligt krav 1 eller 2, k ä n n e t e c k n a t a v att som polyvinylesterdispersion används en polyvinylacetatdis- persion. 7Adhesives according to Claim 1 or 2, characterized in that a polyvinyl acetate dispersion is used as the polyvinyl ester dispersion. 7 4. Lim enligt krav 1 - 3, k ä n n e t e c k n a t a v att som vattenlösligt surt metallsalt används ett salt av aluminium, järn, krom, titan, zirkonium eller vanadin.Adhesives according to Claims 1 to 3, characterized in that a salt of aluminum, iron, chromium, titanium, zirconium or vanadium is used as the water-soluble acid metal salt. 5. Lim enligt krav 1 - 4, k ä n n e t e c k n a t a v att som vattenlösligt, surt metallsalt används aluminiumklorid. - ANFÖRDA PUBLIKATIONER: US 3 311 581 (260-29.4)Adhesives according to claims 1 - 4, characterized in that aluminum chloride is used as the water-soluble, acidic metal salt. - PROMISED PUBLICATIONS: US 3,311,581 (260-29.4)
SE7316881A 1972-12-15 1973-12-13 STORAGE STABLE POLYVINYLESTER-BASED ONE-COMPONENT ADHESIVE CONTAINING POLYVINYL ALCOHOL AS A PROTECTIVE COLOID AND AN URBAN FORMALDEHYDE ADDUCT AND AN ACID METAL SALT SE406330B (en)

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