DK145894B - PROCEDURE FOR THE PREPARATION OF ADDITIVE POLYVINYL ACETATE DISPERSES - Google Patents

PROCEDURE FOR THE PREPARATION OF ADDITIVE POLYVINYL ACETATE DISPERSES Download PDF

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DK145894B
DK145894B DK269576AA DK269576A DK145894B DK 145894 B DK145894 B DK 145894B DK 269576A A DK269576A A DK 269576AA DK 269576 A DK269576 A DK 269576A DK 145894 B DK145894 B DK 145894B
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viscosity
acetate
polyvinyl alcohol
water
resistance
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DK145894C (en
DK269576A (en
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A Caporossi
C Foschi
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Anic Spa
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F18/00Homopolymers and 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
    • C08F18/02Esters of monocarboxylic acids
    • C08F18/04Vinyl esters

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  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
  • Adhesives Or Adhesive Processes (AREA)
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Description

(19) DANMARK(19) DENMARK

© 02) FREMLÆGGELSESSKRIFT <n> 1 it5894 Β© 02) PUBLICATION <n> 1 it5894 Β

DIREKTORATET FOR PATENT- OG VAREMÆRKEVÆSENETDIRECTORATE OF THE PATENT AND TRADEMARKET SYSTEM

(21) Ansøgning nr. 2β95/7β (51) lnt.CI.3 C 08 F 118/08 (22) Indleveringsdag 16. jun. 197^ C 09 J 3/14 (24) Løbedag 16. jun. 1976 (41) Aim. tilgængelig 25« dec. 1976 (44) Fremlagt 5 · apr. 1 983 (86) International ansøgning nr. -(86) International indleveringsdag (85) Videreførelsesdag -(62) Stamansøgning nr. -(21) Application No. 2β95 / 7β (51) lnt.CI.3 C 08 F 118/08 (22) Filing date 16 Jun. 197 ^ C 09 J 3/14 (24) Race day 16 Jun. 1976 (41) Aim. available 25 «dec. 1976 (44) Posted 5 Apr 1 983 (86) International application no. - (86) International filing day (85) Transfer day - (62) Master application no. -

(30) Prioritet 24. jun. 1975, 24703/75, IT(30) Priority Jun 24 1975, 24703/75, IT

(71) Ansøger ANIC S.P.A., Palermo, IT.(71) Applicant ANIC S.P.A., Palermo, IT.

(72) Opfinder Adolfo Caporossi, IT: Claudio Foschi, IT.(72) Inventor Adolfo Caporossi, IT: Claudio Foschi, IT.

(74) Fuldmægtig Internationalt Patent-Bureau.(74) International Patent Bureau.

(54) Fremgangsmåde til fremstilling af som klæbemidler egnede poly= vinylacetatdispersioner.(54) Process for the preparation of adhesives suitable for polyphenyl acetate dispersions.

Opfindelsen angår en fremgangsmåde til fremstilling af som klæbemidler egnede polyvinylacetatdispersioner, specielt sådanne, hvor polyvinylacetatklæbe-stoffet foreligger i en højviskos vandig dispersion og med meget fine polymere partikler, idet man anvender små mængder beskyttende kolloid og ikke anvender overfladeaktive midler.The invention relates to a process for the preparation of adhesive suitable polyvinyl acetate dispersions, especially those wherein the polyvinyl acetate adhesive is present in a highly viscous aqueous dispersion and with very fine polymeric particles, using small amounts of protective colloid and not using surfactants.

® Den udstrakte brug af vandige polyvinylacetatdispersioner er velkendt ved d* . .® The widespread use of aqueous polyvinyl acetate dispersions is well known in the art of d *. .

jj fremstillingen af klæbemidler til træpapir og pap og ved fremstillingen af ag- glomerater af læder, savsmuld, kork og tekstilfibre.in the manufacture of adhesives for wood and cardboard and in the manufacture of agglomerates of leather, sawdust, cork and textile fibers.

OISLAND

3· Det er kendt at fremstille polyvinylacetatklæbestoffer i vandig dispersion ved at anvende beskyttende kolloider, der er opløselige i vand, såsom gummi dj arabicum, methylcellulose, gelatine, stivelse, polyvinylpyrrolidon og polyvinyl- ^ alkohol.3 It is known to prepare polyvinyl acetate adhesives in aqueous dispersion using protective water-soluble colloids such as gum arabic, methyl cellulose, gelatin, starch, polyvinylpyrrolidone and polyvinylalcohol.

2 · 145894 Sædvanligvis anvendes i kommerciel praksis også et emulgerende system, der består af polyvinylalkohol som det beskyttende kolloid i en mængde på fra 5-10% af den totale dispersion, opnået ved alkalisk alkoholyse og med fra 80-90 mol% vinylalkoholenheder med en blokfordeling af den resterende acetylgruppe, sammen med et anionisk eller ikke-ionisk overfladeaktivt middel i en mængde på fra 0,5% op til maksimalt 1,5%. Polyvinylalkohol, der er opnået ved sur alkoholyse og har fra 80-90 mol% vinylalkoholgrupper med en tilfældig og uorganiseret fordeling af acetylgrupperne, anvendes derimod sædvanligvis ikke, da de dispersioner, der opnås med denne slags polyvinylalkohol, giver meget dårlige rheolo-giske- og klæbende egenskaber.2 · 145894 Usually, in commercial practice, an emulsifying system consisting of polyvinyl alcohol as the protective colloid in an amount of from 5-10% of the total dispersion obtained by alkaline alcoholysis and with from 80-90 mole% of vinyl alcohol units having a block distribution of the remaining acetyl group, together with an anionic or nonionic surfactant in an amount of from 0.5% up to a maximum of 1.5%. However, polyvinyl alcohol obtained by acid alcoholysis having from 80-90 mole% vinyl alcohol groups with a random and disorganized distribution of the acetyl groups is not usually used, since the dispersions obtained with this kind of polyvinyl alcohol give very poor rheological and adhesive properties.

Sædvanligvis kræves der for de polyvinylacetatdispersioner, der skal anvendes som klæbestoffer, en meget høj viskositet af den endelige formulering, når den skal anvendes til praktiske formål.Usually, for the polyvinyl acetate dispersions to be used as adhesives, a very high viscosity of the final formulation is required when it is to be used for practical purposes.

Dispersionernes høje viskositet opnås ifølge velkendt teknik ved at forøge mængden af beskyttende kolloid: Dette giver imidlertid dispersioner, der har en meget høj enhedspris,og som udviser klæbeegenskaber, der ikke altid er acceptable, såsom en langsom hærdetid og en lang åbentid. Yderligere'diar det beskyttende kolloid en negativ indflydelse på modstandsdygtigheden af filmen over for vand.The high viscosity of the dispersions is achieved in the prior art by increasing the amount of protective colloid: however, it provides dispersions which have a very high unit price and exhibit adhesive properties which are not always acceptable, such as a slow cure time and a long open time. Further, the protective colloid would adversely affect the film's water resistance.

Af disse grunde er det ønskeligt at holde koncentrationen af det kolloid, der skal anvendes, på det lavest mulige niveau, men idet man gør dette, fås der dispersioner med dårlige egenskaber, idet produktet har tendens til at klumpe efter en lang lagringstid, udviser lav viskositet og en begrænset modstandsdygtighed over for mekaniske og varmepåvirkninger, idet størrelsen af de polymere partikler er stor>med betydelig klumpning.For these reasons, it is desirable to keep the concentration of the colloid to be used at the lowest possible level, but in doing so, dispersions with poor properties are obtained as the product tends to clump after a long storage time, exhibits low viscosity and a limited resistance to mechanical and heat stresses, the size of the polymeric particles being large> with considerable clumping.

Anvendelsen af overfladeaktive midler giver polymerpartikler, der i gennemsnit er små og inden for et begrænset område, men som har lav viskositet og dårlige klæbeegenskaber.The use of surfactants produces polymer particles which are on average small and within a limited range, but which have low viscosity and poor adhesive properties.

Det er klart, at udvælgelsen af emulgeringsmiddel-beskyttelseskolloidsy-sternet i korrekte forhold har en fundamental indflydelse på dispersionernes egenskaber både med hensyn til, hvorledes de opfører sig rheologisk, og ud fra et økonomisk synspunkt.It is clear that the selection of the emulsifier-protecting colloid system in correct conditions has a fundamental influence on the properties of the dispersions both in terms of their rheological behavior and from an economic point of view.

De mest almindeligt anvendte initiatorer ved produktionen af polyvinylacetatdispersioner er vandopløselige og fri radikalproducerende forbindelser, såsom ammonium- eller kaliumpersulfat og hydrogenperoxid.The most commonly used initiators in the production of polyvinyl acetate dispersions are water-soluble and free radical-producing compounds such as ammonium or potassium persulfate and hydrogen peroxide.

Der anvendes oxidations-reduktionssystemer for at give en kortere reaktionstid. Disse systemer består af koblet med zirikformaldehydsulfoxylat, med jernchlorid og ascorbinsyre, ammoniumpersulfat og natriumbisulfit, med tert.-butylhydroperoxid og zinkformaldehydsulfoxylat.Oxidation-reduction systems are used to give a shorter reaction time. These systems consist of coupled with zirconium formaldehyde sulfoxylate, with iron chloride and ascorbic acid, ammonium persulfate and sodium bisulfite, with tert-butyl hydroperoxide and zinc formaldehyde sulfoxylate.

De dispersioner, der opnås i kommerciel praksis, udviser imidlertid stadig 3 U 5894 partikelstørrelser i området 5.000 indtil 50.000 A°-enheder (dvs. et meget stort størrelsesområde for hver dispersion) og stadig en stor procentdel af store partikler. De udviser yderligere begrænset modstandsdygtighed over for mekaniske og termiske påvirkninger, dårlig modstandsdygtighed over for lagring, en klæbeevne, der ikke overskrider 130 kg/cm , og en forholdsvis høj' enhedspris på grund af den store procentdel beskyttende kolloider.However, the dispersions obtained in commercial practice still exhibit 3 U 5894 particle sizes in the range of 5,000 to 50,000 A ° units (i.e., a very large size range for each dispersion) and still a large percentage of large particles. They further exhibit limited resistance to mechanical and thermal stresses, poor resistance to storage, an adhesive capacity not exceeding 130 kg / cm, and a relatively high unit price due to the high percentage of protective colloids.

Det har nu overraskende vist sig, at det er muligt at overvinde disse ulemper ved den tidligere kendte teknik, og opnå meget stabile højviskose polymere dispersioner med meget fine partikler (størrelsen af hver dispersion overstiger ikke 12.000 A°-enheder med et forhold mellem minimum- og maksianumstørrel- 2 sen aldrig under 1/6), en klæbeevne, der er større end 180 kg/cm , en høj modstandsdygtighed både over for mekaniske og termiske påvirkninger, ingen klumpdannelse, film, der er mere homogene og vandtætte, en høj stabilitet af dispersionen, når pH varieres, og en lav produktionspris.It has now surprisingly been found that it is possible to overcome these disadvantages of the prior art and to obtain very stable high viscous polymeric dispersions with very fine particles (the size of each dispersion does not exceed 12,000 A ° units with a ratio of minimum and the maximum size 2 never below 1/6), an adhesive greater than 180 kg / cm, a high resistance to both mechanical and thermal stresses, no lump formation, films that are more homogeneous and waterproof, high stability of the dispersion when pH is varied and a low production cost.

Fremgangsmåden ifølge opfindelsen er af den omtalte kendte art, ved hvilken vinylacetat polymeriseres i vandig dispersion ved konventionel temperatur og i nærværelse af polyvinylalkohol samt et oxiderende og reducerende system, og fremgangsmåden er ejendommelig ved, at det oxiderende system består af hydrogen-peroxid og/eller ammonium-, et alkalimetal- og/eller jordalkalimetalpersulfat i en mængde på fra 0,1-1% af vægten af den totale dispersion,medens det reducerende system består af myresyre,vinsyre,maleinsyre og/eller oxalsyre i en mængde på fra 0,3-0,7% af vægten af den totale dispersion, og at polyvinylalkoholen anvendes i en mængde på 1-5%, beregnet på den totale dispersion, samt at polymeriseringen yderligere foregår i nærværelse af a) et acetat og/eller et sulfat af et grundstof af gruppen VIII i det periodiske system i en mængde på 0,0001-0,005%, beregnet på vægten af den monomere, b) et bicarbonat og/eller et acetat af et alkalieller jordalkalimetal, der tilføres kontinuerligt under polymeriseringsprocessen i en mængde på fra 0,05-0,5%, beregnet på vægten af den monomere, og c) et modificeringsmiddel, valgt blandt aldehyder med kogepunkt under 70°C eller blandt estere af butylalkoholer med kogepunkt over 150° C, i en mængde på mellem 0,01 og 0,5%, beregnet på vægten af den monomere.The process according to the invention is of the prior art in which vinyl acetate is polymerized in aqueous dispersion at conventional temperature and in the presence of polyvinyl alcohol and an oxidizing and reducing system, and the process is characterized in that the oxidizing system consists of hydrogen peroxide and / or ammonium, an alkali metal and / or alkaline earth metal persulfate in an amount of from 0.1 to 1% by weight of the total dispersion, while the reducing system consists of formic acid, tartaric acid, maleic acid and / or oxalic acid in an amount of from 0, 3-0.7% by weight of the total dispersion and the polyvinyl alcohol being used in an amount of 1-5%, based on the total dispersion, and the polymerization being further carried out in the presence of a) an acetate and / or a sulfate of an element of group VIII of the periodic table in an amount of 0.0001-0.005%, based on the weight of the monomer, b) a bicarbonate and / or acetate of an alkaline earth alkaline metal which is fed continuously t during the polymerization process in an amount of 0.05-0.5%, based on the weight of the monomer, and c) a modifier selected from aldehydes having a boiling point below 70 ° C or from esters of butyl alcohols having a boiling point above 150 ° C , in an amount of between 0.01 and 0.5%, based on the weight of the monomer.

Grundstoffet fra gruppen VIII i det periodiske system er især Fe eller Co, fortrinsvis cobalt.The element of Group VIII of the Periodic Table is in particular Fe or Co, preferably cobalt.

Som modificeringsmiddel anvendes især propionaldehyd, acetaldehyd, croton-aldehyd, butyraldehyd eller butylglycolat.Particularly used as a modifier is propionaldehyde, acetaldehyde, croton aldehyde, butyraldehyde or butyl glycolate.

Polyvinylalkohol kan anvendes, hvadenten det er opnået ved sur alkoholyse eller alkalisk alkoholyse.Polyvinyl alcohol can be used, whether obtained by acid alcohol or alkaline alcoholysis.

Bicarbonatet eller acetatet af et alkalimetal eller et alkalijordmetal er især et bicarbonat eller acetat af Na eller K. Bicarbonatet og/eller acetatet tilføres som ovenfor beskrevet kontinuert, hvilket er et særligt overraskende aspekt af fremgangsmåden ifølge opfindelsen, ved hvilken alle andre komponenter 4 145894 i modsætning hertil tilføres reaktoren på en gang.In particular, the bicarbonate or acetate of an alkali metal or alkaline earth metal is a bicarbonate or acetate of Na or K. The bicarbonate and / or acetate is continuously fed as described above, which is a particularly surprising aspect of the process of the invention, in which all other components of in contrast, the reactor is fed at once.

Det er interessant at se, at polyvinylalkoholen, således som den anvendes ifølge den foreliggende opfindelse, forbliver bundet til polymeren med en kemisk binding på grund af en podningsreaktion med vinylacetat.It is interesting to see that the polyvinyl alcohol, as used in the present invention, remains bound to the polymer with a chemical bond due to a grafting reaction with vinyl acetate.

Den således opnåede dispersion udviser ud over de ovennævnte karakteristika, indhold af tørstof på fra 35% til 60 vægt% med en viskositet indtil 50.000 cP.The dispersion thus obtained exhibits, in addition to the above characteristics, a dry matter content of from 35% to 60% by weight with a viscosity up to 50,000 cP.

Udførelse af polymerisationer af vinylacetat i nærværelse af visse af de angivne tilsætninger er i forvejen kendt, men derimod ikke anvendelsen af alle disse tilsætninger samtidig, og i de angivne mængdeforhold, med henblik på fremstilling af som klæbemidler særligt velegnede dispersioner.Carrying out polymerizations of vinyl acetate in the presence of some of the additives disclosed is known in the past, but not the use of all these additives at the same time, and in the stated proportions, for the preparation of particularly suitable dispersions as adhesives.

Således kendes fra beskrivelsen til US-patent nr. 2.965.623 en fremgahgs-- måde til polymerisation af vinylestere i nærværelse af et dobbelt oxidationssystem, nemlig et lipofilt og et hydrofilt peroxid, og i nærværelse af polyvinyl-"alkohol, et aldehyd og et alkalimetalhydroxid eller -carbonat. Det tilsigtes ved denne fremgangsmåde at fremstille polymer-partikler, som har overflader, der modvirker agglomeration og således ikke er egnet til klæbeformål.Thus, from the disclosure of U.S. Patent No. 2,965,623, a method of polymerizing vinyl esters is known in the presence of a dual oxidation system, namely a lipophilic and a hydrophilic peroxide, and in the presence of polyvinyl alcohol, an aldehyde and It is intended in this process to prepare polymer particles having surfaces which resist agglomeration and are thus not suitable for adhesive purposes.

Endvidere kendes fra tysk fremlæggelsesskrift nr. 1.Ό72.813 en fremgangsmåde til fremstilling af stabile, vandige dispersioner af vinylestere i nærværelse af vandopløselige aktivatorer, beskyttelseskolloider og anionaktive emulgatorer. Som aktivator kan anvendes et vandopløseligt peroxid, såsom hydrogenperoxid eller et persulfat, og der tilsættes eventuelt et reduktionsmiddel, såsom vinsyre. Som béSkyttelseskolloid benyttes eksempelvis polyvinylalkohol. Yderligere kan polymerisationen udføres i nærværelse af cobaltacetat, men det essentielle i denne fremgangsmåde er udførelse af fremgangsmåden i nærværelse af salte af metaller fra gruppe II i det periodiske system, især calcium og magnesium, eller af aluminium. Formålet med denne sidste tilsætning,! kombination med anionaktiv emulgator, er at opnå en dispersion med nogenlunde ensartede,små partikelstørrelser, som er velegnet for fremstilling af homogene glasklare, glinsende og glatte film og derfor heller ikke må have høj viskositet, men skal have gode flydeegenskaber af hensyn til den lette udstrygning og sammenflydning.Furthermore, from German Patent Specification No. 1,772,813, a process is known for preparing stable aqueous dispersions of vinyl esters in the presence of water-soluble activators, protective colloids and anion-active emulsifiers. As an activator, a water-soluble peroxide such as hydrogen peroxide or persulfate may be used, and optionally a reducing agent such as tartaric acid is added. As a protective colloid, for example, polyvinyl alcohol is used. Further, the polymerization may be carried out in the presence of cobalt acetate, but the essential in this process is the execution of the process in the presence of Group II metals salts in the periodic table, especially calcium and magnesium, or of aluminum. The purpose of this last addition,! combination with anion-active emulsifier, is to obtain a dispersion of fairly uniform, small particle sizes suitable for the preparation of homogeneous clear, shiny and smooth films and therefore must not have high viscosity, but must have good flow properties for ease of ironing. and confluence.

Ved fremgangsmåden ifølge den foreliggende opfindelse anvendes ikke en kombination af anionaktiv emulgator og calcium-, magnesium- eller aluminiumsalt som angivet i det tyske fremlæggelsesskrift.In the process of the present invention, a combination of anion-active emulsifier and calcium, magnesium or aluminum salt as used in the German disclosure is not used.

Som tidligere angivet bidrager anvendelsen af overfladeaktive midler almindeligvis til opnåelsen af lav viskositet og dårlige klæbeegenskaber. I det foreliggende tilfælde tilsigtes der netop, som tidligere nævnt, opnået højviskose dispersioner med meget fine partikler og stor klæbeevne. Ved fremgangsmåden ifølge opfindelsen kan der, som det vil fremgå af de efterfølgende udførelseseksemp-As previously stated, the use of surfactants generally contributes to the attainment of low viscosity and poor adhesive properties. In the present case, just as previously mentioned, high viscous dispersions with very fine particles and high adhesiveness are intended. In the method according to the invention, as will be apparent from the following embodiments,

U539AU539A

5 ler, opnås partikler med størrelser, der er lavere end de i det tyske fremlæggelsesskrift angivne, samtidig med stor klæbeevne.5 clay, particles with sizes lower than those specified in German disclosure are obtained, together with high adhesive properties.

I det følgende anføres de metoder, der er anvendt til karakterisering af de således opnåede dispersioner, hvis fremstilling er omtalt i eksemplerne, fremgangsmåder til karakterisering.In the following, the methods used to characterize the dispersions thus obtained, the preparation of which are discussed in the Examples, are described methods of characterization.

1. Partikelstørrelse.1. Particle size.

Partikelstørrelsen af polyvinylacetatdispersionen og dens fordelingsområde undersøges i mikroskop med inddelt okular, og idet dispersionen først fortyndes med vand.The particle size of the polyvinyl acetate dispersion and its distribution range is examined in a divided eyepiece microscope and the dispersion first diluted with water.

2. Klæbeevne.2. Adhesiveness.

Modstandsdygtigheden mod ophævelse af klæbningen bestemmes på sammenlimede ahornprøver. Prøven udføres på en trækprøvemaskine.The resilience of removing the adhesive is determined on glued maple samples. The test is performed on a tensile tester.

3. Bestandighed over for frysning og optøning.3. Resistance to freezing and thawing.

Prøven indføres i en termostatisk celle, der er programmeret til en vis cyclus. Sædvanligvis er der fem cycler, som går fra -12°C til +20°C. Hver cyclus varer 12 timer. Efter afslutningen af hver cyclus måles viskositeten af dispersionen.The sample is introduced into a thermostatic cell programmed for a certain cycle. Usually there are five cycles ranging from -12 ° C to + 20 ° C. Each cycle lasts 12 hours. At the end of each cycle, the viscosity of the dispersion is measured.

4. Mekanisk stabilitet.4. Mechanical stability.

Prøven har til hensigt at måle viskositetsnedgangene på grund af hurtig omrøring, forskydningsspændinger, vridninger, lamineringer og pumpninger. Produktet underkastes kraftig omrøring ved hjælp af en turbodisperser ved 1500 omdrejninger. Efter 24 timers henstand aflæses viskositeten.The test intends to measure the viscosity decreases due to rapid agitation, shear stresses, torsions, laminations and pumps. The product is subjected to vigorous stirring by means of a turbocharger at 1500 rpm. After 24 hours standing, the viscosity is read.

5. Måling af bundfald.5. Measurement of precipitation.

Dispersionen fortyndes med vand og filtreres herefter gennem en si, der har maskestørrelse på 0,15 mm. Værdien udtrykkes i mg/kg (mg/kg).The dispersion is diluted with water and then filtered through a sieve having a mesh size of 0.15 mm. The value is expressed in mg / kg (mg / kg).

6. Bestandighed ved accelereret lagring.6. Resistance to accelerated storage.

Dispersionen holdes i en ovn ved 50°C i 30 dage, hvorefter begyndelses-og s lutviskositeten sammenlignes.The dispersion is kept in an oven at 50 ° C for 30 days, after which the initial and s lute viscosity are compared.

7. Viskositet.7. Viscosity.

Viskositeten måles ved 20°C med et HAT Brookfield viskosimeter med en hastighed på 20 omdrejninger. Aflæsningerne udtrykkes i centipoises (cP).The viscosity is measured at 20 ° C with a HAT Brookfield viscometer at a speed of 20 rpm. The readings are expressed in centipoises (cP).

8. Faste stoffer.8. Solids.

Tørvægtsprocenten bestemmes efter at have tørret dispersionen i en ovn ved 220°C i 15-20 minutter.The dry weight percentage is determined after drying the dispersion in an oven at 220 ° C for 15-20 minutes.

9. pH.9. pH.

Aflæsningerne foretages ved 20°C på et pH-meter.The readings are made at 20 ° C on a pH meter.

6 1458946 145894

Eksempel 1 (fremstillet som sammenligning)Example 1 (prepared by comparison)

Vand 1.200 gramWater 1,200 grams

Delvist forsæbet polyvinylalkohol (alkalisk alkoholyse) 115 ”Partially saponified polyvinyl alcohol (alkaline alcoholysis) 115 ”

Natriumdodecylbenzensulfonat 6,5 "Sodium dodecylbenzenesulfonate 6.5 "

Vinylacetat 1.250 "Vinyl Acetate 1,250 "

Hydrogénperoxid (35%) 25 11Hydrogen Peroxide (35%) 11

En rustfri stålreaktor udstyret med e.n ankerformet omrører, der kører med 100 omdrejninger, og en reflux-kondensator tilsættes vand, polyvinylalkohol, natriumdodecylbenzensulfonat, der først er opløst i vand, hydrogenperoxid og 450 g vinylacetat. Blandingen opvarmes til 68°C, og polymerisationen udføres ved at tilføre den resterende vinylacetat i løbet af 4 timer. Under polymerisationsreaktionen bør temperaturen holdes på ca. 68°C til 70°C.A stainless steel reactor equipped with an anchor-shaped stirrer running at 100 rpm and a reflux condenser are added to water, polyvinyl alcohol, sodium dodecylbenzenesulfonate first dissolved in water, hydrogen peroxide and 450 g vinyl acetate. The mixture is heated to 68 ° C and the polymerization is performed by adding the remaining vinyl acetate over 4 hours. During the polymerization reaction, the temperature should be kept at approx. 68 ° C to 70 ° C.

Karakteristik.Characteristics.

Faste stoffer 50,3%Solids 50.3%

Viskositet 3.400 cPViscosity 3,400 cP

pH 4,35pH 4.35

Bundfald 150 dele pr. million 2Precipitation 150 parts per million 2

Klæbeevne 135 kg/cmAdhesive capacity 135 kg / cm

Frysning-optøningscycler fortykker ved anden cyclusFreeze-thaw cycles thicken by the second cycle

Partikelstørrelse (5% med ca. 50.000 Å-enheder (70% » » 30.000 " (25% » " 10.000 » (nogle få klumperParticle size (5% with about 50,000 Å units (70% »» 30,000 "(25%» "10,000" (a few lumps)

Mekanisk stabilitet dårligMechanical stability poor

Lagringsbestandighed dårligStorage resistance poor

Eksempel 2Example 2

Vand 1.200 gramWater 1,200 grams

Delvis forsæbet (alkalisk alkoholyse) polyvinylalkohol 65 11Partially saponified (alkaline alcoholysis) polyvinyl alcohol 65 11

Vinylacetat 1.250 "Vinyl Acetate 1,250 "

Natriumperoxid 15 "Sodium Peroxide 15 "

Myresyre 12 ”Formic acid 12 ”

Manganacetat 0,1 "Manganese acetate 0.1 "

Ammoniumpersulfat 2Ammonium persulfate 2

Natriumcarbonat 27 ”Sodium carbonate 27 "

Acetaldehyd (et modificeringsmiddel) 13 " 900 g vand tilsættes polyvinylalkohol, der allerede er opløst, natriumperoxid, myresyre og manganacetat, ammoniumpersulfat og 250 g vinylacetat. Blandingen opvarmes til 68°C, og polymeriseringen udføres ved at tilføre de anførte 7 145894 mængder af vinylacetat, vand og natriumcarbonat i løbet af 3 timer.Acetaldehyde (a modifier) 13 "900 g of water is added to the already dissolved polyvinyl alcohol, sodium peroxide, formic acid and manganese acetate, ammonium persulfate and 250 g of vinyl acetate. , water and sodium carbonate over 3 hours.

Under polymeriseringen bør temperaturen holdes på ca. 75-80°C. Karakteristik.During the polymerization, the temperature should be kept at approx. 75-80 ° C. Characteristics.

Faste stoffer 49,97»Solids 49.97 »

Viskositet 27.000 cPViscosity 27,000 cP

pH 4,75pH 4.75

Bundfald 73 dele pr. million 2Precipitation 73 parts per million 2

Klæbeevne 198 kg/cmAdhesive capacity 198 kg / cm

Frysnings-optøningscycler uændretFreeze-thaw cycles unchanged

Partikelstørrelse (10% med ca. 10.000 Å-enheder (90% ·' «· 5.000 '< (ingen klumpningParticle size (10% with about 10,000 Å units (90% · '' · 5,000 '<(no clumping)

Mekanisk stabilitet særdeles godMechanical stability very good

Lagringsbestandighed " "Storage resistance ""

Eksempel 3Example 3

Vand 1.400 gramWater 1,400 grams

Delvis forsæbet (alkalisk alkoholyse) polyvinylalkohol 95 "Partially saponified (alkaline alcoholysis) polyvinyl alcohol 95 "

Vinylacetat 900 " 35%-hydrogenperoxid 28 " V insyre 8 *’Vinyl Acetate 900 "35% Hydrogen Peroxide 28" V Acetic Acid 8 * '

Cobaltacetat 0,16Cobalt acetate 0.16

Kaliumpersulfat 2 "Potassium persulfate 2 "

Natriumbicarbonat 21 MSodium bicarbonate 21 M

Butylacetat 63 ”Butyl acetate 63 ”

Polymerisering.Polymerization.

Fremgangsmåden er den samme som i eksempel 2 med 500 g vand, 600 g vinylacetat og natriumbicarbonat, der tilføres. Reaktionstemperaturen er 75-85°C. Karakteristik.The procedure is the same as in Example 2 with 500 g of water, 600 g of vinyl acetate and sodium bicarbonate added. The reaction temperature is 75-85 ° C. Characteristics.

Faste stoffer 36,37.Solids 36.37.

Viskositet 30.500 cPViscosity 30,500 cP

pH 4,75pH 4.75

Bundfald 28 dele pr. million 2Precipitation 28 parts per million 2

Klæbeevne 191 kg/cmAdhesive capacity 191 kg / cm

Frysnings-optøningscycler uændretFreeze-thaw cycles unchanged

Partikelstørrelse (20% med ca. 10,000 Å-enheder (80% » » ‘5.000 » (ingen klumpningParticle size (20% with about 10,000 Å units (80% »» '5,000 »(no clumping)

Mekanisk stabilitet særdeles godMechanical stability very good

Lagringsbestandighed " " 8 145894Storage Resistance "" 8 145894

Eksempel 4Example 4

Vand 900 gramWater 900 grams

Delvis forsæbet (alkalisk alkoholyse) polyvinylalkohol 25 "Partially saponified (alkaline alcoholysis) polyvinyl alcohol 25 "

Delvis forsæbet (sur alkoholyse) polyvinylalkohol 25 n 35% hydrogenper oxid 14 11Partially saponified (acid alcoholysis) polyvinyl alcohol 25 n 35% hydrogen per oxide 14 11

Kaliumpersulfat 2,2 MPotassium persulfate 2.2 M

Ferrosulfat (der erstatterFerrosulphate (replacing

Co-acetat) 0,15 "Co-acetate) 0.15 "

Butylbutyrat 29 11Butyl Butyrate 29 11

Vinylacetat 1500 ”Vinyl acetate 1500 ”

Maleinsyre (der erstatter H-C00H) 13 "Maleic acid (replacing H-C00H) 13 "

Natriumacetat (der erstatter Na- bicarbonat) 23 !tSodium acetate (replacing Na- bicarbonate) 23 hours

Polymerisering.Polymerization.

Fremgangsmåden er den samme som i eksempel 2. Reaktionstemperaturen er 75-85°C.The procedure is the same as in Example 2. The reaction temperature is 75-85 ° C.

Karakteristik.Characteristics.

Faste stoffer 60,7%Solids 60.7%

Viskositet 33.000 cPViscosity 33,000 cP

pH 4,65pH 4.65

Bundfald 37 dele pr. million 2Precipitation 37 parts per million 2

Klæbeevne 206 kg/cmAdhesive capacity 206 kg / cm

Frysnings-optøningscycler uændretFreeze-thaw cycles unchanged

Partikelstørrelse (100% med ca. 5.000 Å-enheder ( ingen klumperParticle size (100% with about 5,000 Å units (no lumps)

Mekanisk stabilitet særdeles godMechanical stability very good

Lagringsbestandighed " 11Storage resistance "11

Eksempel 5Example 5

Vand 1.000 gramWater 1,000 grams

Delvis forsæbet (sur alkoholyse) polyvinylalkohol 71 11Partially saponified (acid alcoholysis) polyvinyl alcohol 71 11

Vinylacetat 1.350 "Vinyl Acetate 1.350 "

Natriumperoxid 19 "Sodium Peroxide 19 "

Vinsyre 12 "Tartaric Acid 12 "

Cobaltacetat 0,11 MCobalt acetate 0.11 M

Ammoniumpersulfat 7 "Ammonium persulfate 7 "

Grotonaldehyd 18 11Grotonaldehyde 18 11

Natriumbicarbonat 18 Tl 9 1Α589ΛSodium bicarbonate 18 Tl 9 1Α589Λ

Polymerisering.Polymerization.

Fremgangsmåden er den samme som i eksempel 3. Reaktionstemperaturen er 75-85°C.The procedure is the same as in Example 3. The reaction temperature is 75-85 ° C.

Karakteristik.Characteristics.

Faste stoffer 53,3%Solids 53.3%

Viskositet 41.500 cPViscosity 41,500 cP

pH 4,7pH 4.7

Bundfald 52 dele pr. million 2Precipitation 52 parts per million 2

Klæbeevne 200 kg/cmAdhesive capacity 200 kg / cm

Frysnings-optøningscycler uændretFreeze-thaw cycles unchanged

PartikelstørreIse (100% med ca. 3.000 Å-enheder (ingen klumpningParticle size (100% with about 3,000 Å units (no clumping)

Mekanisk stabilitet særdeles godMechanical stability very good

Lagringsbestandighed 11 nStorage resistance 11 n

Eksempel 6Example 6

Vand 1.200 gramWater 1,200 grams

Delvis forsæbet (alkalisk alkoholyse) polyvinylalkohol 75 MPartially saponified (alkaline alcoholysis) polyvinyl alcohol 75 M

Vinylacetat 1.250 n 35% hydrogenperoxid 22 11Vinyl acetate 1,250 n 35% hydrogen peroxide 22 11

Myresyre 12 nFormic acid 12 n

Gobaltacetat 0,33 gram K-persulfat 1,5 "Gobalt acetate 0.33 grams K-persulfate 1.5 "

NaHC03 30 » 900 g vand tilsættes polyvinylalkohol, der først er opløst, hydrogenper-oxid, myresyre, cobaltacetat, K-persulfatet og 250 g vinylacetat. Blandingen opvarmes til 68°G, qg polymeriseringen udføres ved at tilføre de anførte mængder af vinylacetat, vand og NaHCO^ i løbet af 3 timer. Under polymeriseringen bør temperaturen holdes på ca. 75-80°C.NaHCO3 30 »900 g of water are added first dissolved polyvinyl alcohol, hydrogen peroxide, formic acid, cobalt acetate, K-persulfate and 250 g vinyl acetate. The mixture is heated to 68 ° G, and the polymerization is carried out by adding the indicated amounts of vinyl acetate, water and NaHCO3 over 3 hours. During the polymerization, the temperature should be kept at approx. 75-80 ° C.

Karakteristik.Characteristics.

Faste stoffer 50,1%Solids 50.1%

Viskositet 37.000 cPViscosity 37,000 cP

pH 3,75pH 3.75

Bundfald 73 dele pr. million 2Precipitation 73 parts per million 2

Klæbeevne 198 kg/cmAdhesive capacity 198 kg / cm

Frysnings-opløsningscycler uændretFreeze-dissolution cycles unchanged

Partikelstørrelse (10% med ca. 10.000 Å-enheder (90% '' » 5.000 << (nogle få klumper 145894 ίοParticle size (10% with about 10,000 Å units (90% '' '5,000 << (a few clumps 145894 ίο

Bestandighed over for mekaniske påvirk- middelgod viskositet ned- ninger sættes med 25%Resistance to mechanical impact good viscosity decreases by 25%

Lagringsbestandighed særdeles godStorage resistance very good

Eksempel 7Example 7

Vand 1.400 gramWater 1,400 grams

Delvis forsæbet (alkalisk alkoholyse) polyvinylalkohol 100 "Partially saponified (alkaline alcoholysis) polyvinyl alcohol 100 "

Vinylacetat 900 " 35% hydrogenperoxid 28 "Vinyl Acetate 900 "35% Hydrogen Peroxide 28"

Myresyre 12 "Formic acid 12 "

Gobaltacetat 0,33 " K-persulfat 1,3 "Gobalt acetate 0.33 "K-persulfate 1.3"

NaHCO^ 22 »'NaHCO2 22

Polymerisering.Polymerization.

Fremgangsmåden er den samme som i eksempel 2, idet der kontinuerligt tilføres 500 g vand og 600 g vinylacetat og NaHC0„. Reaktionstemperaturen er 75-85 °G.The procedure is the same as in Example 2, continuously adding 500 g of water and 600 g of vinyl acetate and NaHCO The reaction temperature is 75-85 ° G.

Karakteristik.Characteristics.

Faste stoffer 36,3%Solids 36.3%

Viskositet 30.500 cPViscosity 30,500 cP

pH 4,75pH 4.75

Bundfald 28 dele pr. million 2Precipitation 28 parts per million 2

Klæbeevne 191 kg/cmAdhesive capacity 191 kg / cm

Frysning s-optønings cycler uændretFreezing s-thaw cycles unchanged

Partikelstørrelse (20% med ca. 5.000 Å (80% » » 3.000 Å (nogle få klumperParticle size (20% by about 5,000 Å (80%) »» 3,000 Å (a few lumps)

Bestandighed over for mekaniske påvirkninger godResistance to mechanical stresses good

Lagringsbestandighed '*Storage Resistance '*

Eksempel 8Example 8

Vand 1.400 gramWater 1,400 grams

Delvis forsæbet (alkalisk alkoholyse) polyvinylalkohol 115 "Partially saponified (alkaline alcoholysis) polyvinyl alcohol 115 "

Vinylacetat 900 " 35% hydrogenperoxid 31 *'Vinyl Acetate 900 "35% Hydrogen Peroxide 31"

Myresyre 12 "Formic acid 12 "

Cobaltacetat 0,33 " 1Λ5894 11 K-persulfat 1,3 11Cobalt Acetate 0.33 "1.5894 11 K Persulfate 1.3 11

NaHC03 22 »'NaHC03 22 »'

Butylglycolat 50 "Butyl Glycolate 50 "

Polymerisering.Polymerization.

Fremgangsmåden er den samme som i eksempel 3. Reaktionstemperaturen 75-85°C.The procedure is the same as in Example 3. The reaction temperature is 75-85 ° C.

Karakteristik.Characteristics.

Faste stoffer 35,9%Solids 35.9%

Viskositet 31.000 cPViscosity 31,000 cP

pH 4,65pH 4.65

Bundfald 37 dele pr. million 2Precipitation 37 parts per million 2

Klæbeevne 206 kg/cmAdhesive capacity 206 kg / cm

Frysnings-optøningscycler uændretFreeze-thaw cycles unchanged

PartikelstørreIse (100% med ca. 3.000 AParticle size (100% with about 3,000 A

(ingen klumper(no lumps

Bestandighed over for mekaniske på- særdeles god - ingen viskosi- virkninger tetsændringerResistance to mechanical extremely good - no viscosity effects

Lagringsbestandighed meget god - ingen viskosi tetsændringerStorage resistance very good - no viscosity changes

Eksempel 9Example 9

Vand 1.200 gramWater 1,200 grams

Delvis forsæbet (alkalisk alkoholyse) polyvinylalkohol 84 "Partially saponified (alkaline alcoholysis) polyvinyl alcohol 84 "

Vinylacetat 1.250 MVinyl acetate 1,250 M

35% hydrogenperoxid 24 "35% hydrogen peroxide 24 "

Myresyre 12 nFormic acid 12 n

Cobaltacetat 0,33 " K-persulfat 1,3 11Cobalt Acetate 0.33 "K Persulfate 1.3 11

NaHCOg 30 »NaHCOg 30 »

Propionaldehyd 10 "Propionaldehyde 10 "

Polymerisering.Polymerization.

Fremgangsmåden er den samme som i eksempel 2. Reaktionstemperatur 75-85°C. Karakteristik.The procedure is the same as in Example 2. Reaction temperature 75-85 ° C. Characteristics.

Faste stoffer 50,5%Solids 50.5%

Viskositet 24.000 cPViscosity 24,000 cP

pH 4,7pH 4.7

Bundfald 42 dele pr. million 2Precipitation 42 parts per million 2

Klæbeevne 203 kg/cmAdhesive capacity 203 kg / cm

Frysnings-optøningscycler uændret 12Freeze-thaw cycles unchanged 12

1A589A1A589A

Partikelstørrelse (10% med ca. 5.000 Å-enheder (90% » » 3.000 » (ingen klumpningParticle size (10% with about 5,000 Å units (90% »» 3,000 »(no lumping)

Bestandighed over for mekaniske særdeles god - viskositet påvirkninger uændretResistance to mechanical extremely good - viscosity impacts unchanged

Lagringsbestandighed særdels god - viskositet uændretStorage resistance very good - viscosity unchanged

Eksempel 10Example 10

Vand 1.250 gramWater 1,250 grams

Delvis forsæbet (alkalisk alkoholyse) polyvinylalkohol 79 HPartially saponified (alkaline alcoholysis) polyvinyl alcohol 79 H

Vinylacetat 1.250 n 35% hydrogenperoxid 27 "Vinyl acetate 1,250 n 35% hydrogen peroxide 27 "

Myresyre 12 "Formic acid 12 "

Gobaltacetat 0,33 "Gobalt Acetate 0.33 "

K-persulfat 1,3 MK-persulfate 1.3 M

NaHCOg 30 "NaHCO

Butylglycolat 50 "Butyl Glycolate 50 "

Polymerisering..Polymerization ..

Fremgangsmåden er den samme som i eksempel 2. Reaktionstemperaturen er 75-85°C.The procedure is the same as in Example 2. The reaction temperature is 75-85 ° C.

Karakteristik.Characteristics.

Faste stoffer 49,9%Solids 49.9%

Viskositet 31.000 cPViscosity 31,000 cP

pH 4,7pH 4.7

Bundfald 40 dele pr. million 2Precipitation 40 parts per million 2

Klæbeevne 195 kg/cmAdhesive capacity 195 kg / cm

Frysnings-optøningscycler uændretFreeze-thaw cycles unchanged

Partikelstørrelse ( 5% med ca. 5.000 Å-enheder (95% » » 3.000 » (ingen klumperParticle size (5% with about 5,000 Å units (95% »» 3,000 »(no lumps)

Bestandighed over for mekaniske særdeles god - viskositet påvirkninger uændretResistance to mechanical extremely good - viscosity impacts unchanged

Lagringsbestandighed særdeles god - viskositet uændretStorage resistance extremely good - viscosity unchanged

Eksempel 11Example 11

Vand 1.200 gramWater 1,200 grams

Delvis forsæbet (alkalisk alkoholyse) polyvinylalkohol 84 »Partially saponified (alkaline alcoholysis) polyvinyl alcohol 84 »

Vinylacetat 1.250 " 35% hydrogenperoxid 27 " 145894 13Vinyl acetate 1.250 "35% hydrogen peroxide 27" 13

Myresyre 12 "Formic acid 12 "

Cobaltacetat 0,33 n K-persulfat 1,5 ”Cobalt Acetate 0.33 n K Persulfate 1.5 ”

Natriumacetat 40 "Sodium Acetate 40 "

Propionaldehyd 10 11Propionaldehyde 10 11

Polymerisering.Polymerization.

Fremgangsmåden er den samme som i eksempel 2, idet natriumacetatet tilføres kontinuert. Reaktionstemperaturen er 75-85°C.The procedure is the same as in Example 2, with the sodium acetate being added continuously. The reaction temperature is 75-85 ° C.

Karakteristik.Characteristics.

Faste stoffer 50,7%Solids 50.7%

Viskositet 24.500 cPViscosity 24,500 cP

pH 4,55pH 4.55

Bundfald 78 dele pr. million 2Precipitation 78 parts per million 2

Klæbeevne 188 kg/cmAdhesive capacity 188 kg / cm

Frysnings-optøningscycler fortykner ved den fjerde cyclusFreeze-thaw cycles thicken by the fourth cycle

Partikelstørrelse (10% med ca. 10.000 Å (30% '» '» 7.000 " (60% » » 5.000 » (ingen klumperParticle size (10% by about 10,000 Å (30% "" "" 7,000 "(60%" "5,000" (no lumps)

Bestandighed over for mekaniske særdeles god - viskositet påvirkninger uændretResistance to mechanical extremely good - viscosity impacts unchanged

Lagringsbestandighed dårligStorage resistance poor

Eksempel 12Example 12

Vand 1.200 gramWater 1,200 grams

Delvis forsæbet (alkalisk alkoholyse) polyvinylalkohol 43 "Partially saponified (alkaline alcoholysis) polyvinyl alcohol 43 "

Delvis forsæbet polyvinylalkohol (sur alkoholyse) 43 ”Partially saponified polyvinyl alcohol (acid alcoholysis) 43 ”

Vinylacetat 1.250 " 35% hydrogenperoxid 26,5 "Vinyl Acetate 1,250 "35% Hydrogen Peroxide 26.5"

Myresyre 12Formic acid 12

Cobaltacetat 0,33 " K-persulfat 1,5 "Cobalt Acetate 0.33 "K-Persulfate 1.5"

Propionaldehyd 10 "Propionaldehyde 10 "

NaHC03 27 "NaHCO3 27 "

Polymer is ering.Polymer is herring.

Fremgangsmåden er den samme som i eksempel 2. Reaktionstemperaturen er 75-85°C.The procedure is the same as in Example 2. The reaction temperature is 75-85 ° C.

14 14589614 145896

Karakteristik.Characteristics.

Faste stoffer 50,8%Solids 50.8%

Viskositet 26.500 cPViscosity 26,500 cP

pH 4,75pH 4.75

Bundfald 92 dele pr. million 2Precipitation 92 parts per million 2

Klæbeevne 204 kg/cmAdhesive capacity 204 kg / cm

Frysnings-optøningscycler uændretFreeze-thaw cycles unchanged

Partikelstørrelse (10% med ca. 5.000 Å-enheder (90% » » 3.000 »« (ingen klumperParticle size (10% with about 5,000 Å units (90% »» 3,000 »« (no lumps)

Bestandighed over for mekåniske særdeles god - viskositet påvirkninger uændretResistance to Meccanic extremely good - viscosity impacts unchanged

Lagringsbestandighed særdeles godStorage resistance very good

Eksempel 13Example 13

Vand * 800 gramWater * 800 grams

Delvis forsæbet (sur alkoholyse) polyvinylalkohol 69 "Partially saponified (acid alcoholysis) polyvinyl alcohol 69 "

Vinylacetat 1.250 *'Vinyl Acetate 1,250 * '

35% hydrogenperoxid 25 M35% hydrogen peroxide 25 M

Myresyre 12 gramFormic acid 12 grams

Gobaltacetat 0,33 » K-persulfat 1,5 »Gobalt acetate 0.33 »K-persulfate 1.5»

Pripionaldehyd 10 «Pripionaldehyde 10

NaHC03 22 «NaHCO3 22 «

Polymerisering.Polymerization.

Fremgangsmåden er den samme som i eksempel 2. Reaktionstemperaturen er 75-85°G.The procedure is the same as in Example 2. The reaction temperature is 75-85 ° G.

Karakteristik.Characteristics.

Faste stoffer 60%Solids 60%

Viskositet 25.500 cPViscosity 25,500 cP

pH 4,8pH 4.8

Bundfald 60 dele pr. million 2Precipitation 60 parts per million 2

Klæbeevne 207 kg/cmAdhesive capacity 207 kg / cm

Frysnings-optøningscycler uændretFreeze-thaw cycles unchanged

Partikelstørrelse (100% med ca. 3.000 Å-enheder (ingen klumperParticle size (100% with about 3,000 Å units (no lumps)

Bestandighed over for mekaniske særdeles god - ingen vispåvirkninger kositetsforandringResistance to mechanical extremely good - no visibility effects change in quality

Lagringsbestandighed god 15 U5894Storage resistance good 15 U5894

Eksempel 14Example 14

Vand 800 gramWater 800 grams

Delvis forsæbet (sur alkoholyse) polyvinylalkohol - 60 11Partially saponified (acid alcoholysis) polyvinyl alcohol - 60 11

Vinylacetat 1.250 n 357. hydrogenperoxid 26 ”Vinyl Acetate 1,250 n 357. Hydrogen Peroxide 26 "

Myresyre 12 nFormic acid 12 n

Gobaltacetat 0,33 11 K-persulfat 1,5 nGobalt acetate 0.33 11 K persulfate 1.5 n

NaHC03 22 «NaHCO3 22 «

Butylglycolat 50 nButyl glycolate 50 n

Polymerisering.Polymerization.

Fremgangsmåden er den samme som i eksempel 2. Reaktionstemperaturen er 75-85°C.The procedure is the same as in Example 2. The reaction temperature is 75-85 ° C.

Karakteristik.Characteristics.

Faste stoffer 60,5%Solids 60.5%

Viskositet 29.500 cPViscosity 29,500 cP

pH 4,7pH 4.7

Bundfald 52 dele pr. million 2Precipitation 52 parts per million 2

Klæbeevne 200 kg/cmAdhesive capacity 200 kg / cm

Frysnings-opt^ningscycler uændretFreeze-thaw cycles unchanged

PartikelstørreIse (1007. med ca. 3.000 A-enheder (ingen klumperParticle size (1007. with about 3,000 A units (no lumps)

Bestandighed over for mekaniske særdeles god - viskositet påvirkninger uændretResistance to mechanical extremely good - viscosity impacts unchanged

Lagringsbestandighed godStorage resistance good

DK269576A 1975-06-24 1976-06-16 PROCEDURE FOR THE PREPARATION OF ADDITIVE POLYVINYL ACETATE DISPERSES DK145894C (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
IT2470375 1975-06-24
IT24703/75A IT1039354B (en) 1975-06-24 1975-06-24 PROCEDURE FOR THE PRODUCTION OF POLYACETOVINYL DISPERSIONS AND THUS OBTAINED DISPERSIONS

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JPS57100107A (en) * 1980-12-12 1982-06-22 Daicel Chem Ind Ltd Preparation of adhesive
JPS59109568A (en) * 1982-12-14 1984-06-25 Daicel Chem Ind Ltd High-speed adhesive for paper
CA1261538A (en) * 1984-07-19 1989-09-26 Ronald W. Novak Aldehyde or imine oxygen scavengers for vinyl polymerizations
GB8729702D0 (en) * 1987-12-21 1988-02-03 Unilever Plc Emulsion polymerisation
JP2707597B2 (en) * 1988-05-16 1998-01-28 三井石油化学工業株式会社 Method for producing fluorine-containing polyolefin
DE102006006579A1 (en) * 2006-02-13 2007-08-23 Wacker Polymer Systems Gmbh & Co. Kg Process for the production of molded parts from cork particles
US9733003B2 (en) 2012-12-27 2017-08-15 OXEN, Inc. Ice maker
JP2019031581A (en) * 2015-12-28 2019-02-28 株式会社クラレ Low polymerization degree vinyl alcohol-based polymer powder having excellent color tone and production method thereof
CN108219043A (en) * 2016-12-21 2018-06-29 中国石化集团四川维尼纶厂 A kind of preparation method of polyvinyl acetate emulsion

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NO145577B (en) 1982-01-11
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AT353005B (en) 1979-10-25
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PT65260A (en) 1976-07-01
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ATA458276A (en) 1979-03-15
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PT65260B (en) 1977-12-07
FI61501C (en) 1982-08-10
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