NO150318B - PROCEDURE FOR PREPARING VINYLESTER POLYMER DISPERSIONS - Google Patents
PROCEDURE FOR PREPARING VINYLESTER POLYMER DISPERSIONS Download PDFInfo
- Publication number
- NO150318B NO150318B NO773948A NO773948A NO150318B NO 150318 B NO150318 B NO 150318B NO 773948 A NO773948 A NO 773948A NO 773948 A NO773948 A NO 773948A NO 150318 B NO150318 B NO 150318B
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- Prior art keywords
- acetate
- mixture
- water
- added
- temperature
- Prior art date
Links
- 238000000034 method Methods 0.000 title claims description 15
- 229920001567 vinyl ester resin Polymers 0.000 title claims description 7
- 239000006185 dispersion Substances 0.000 title claims description 6
- 229920000642 polymer Polymers 0.000 title claims description 5
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 claims description 12
- 239000000203 mixture Substances 0.000 claims description 11
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 10
- 239000000178 monomer Substances 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 238000006116 polymerization reaction Methods 0.000 claims description 7
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 6
- BVKZGUZCCUSVTD-UHFFFAOYSA-M Bicarbonate Chemical compound OC([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-M 0.000 claims description 5
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 4
- 230000003647 oxidation Effects 0.000 claims description 4
- 238000007254 oxidation reaction Methods 0.000 claims description 4
- 125000005250 alkyl acrylate group Chemical group 0.000 claims description 3
- UTOVMEACOLCUCK-PLNGDYQASA-N butyl maleate Chemical compound CCCCOC(=O)\C=C/C(O)=O UTOVMEACOLCUCK-PLNGDYQASA-N 0.000 claims description 3
- 125000004432 carbon atom Chemical group C* 0.000 claims description 3
- 239000000084 colloidal system Substances 0.000 claims description 3
- 230000001681 protective effect Effects 0.000 claims description 3
- YGWLMFNSGMKGIB-HJWRWDBZSA-N 1-o-ethyl 4-o-hexyl (z)-but-2-enedioate Chemical compound CCCCCCOC(=O)\C=C/C(=O)OCC YGWLMFNSGMKGIB-HJWRWDBZSA-N 0.000 claims description 2
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 2
- 239000013543 active substance Substances 0.000 claims description 2
- 239000000654 additive Substances 0.000 claims description 2
- 229910052783 alkali metal Inorganic materials 0.000 claims description 2
- 150000001340 alkali metals Chemical class 0.000 claims description 2
- 229910052784 alkaline earth metal Inorganic materials 0.000 claims description 2
- 150000001342 alkaline earth metals Chemical class 0.000 claims description 2
- 125000000217 alkyl group Chemical group 0.000 claims description 2
- 239000012736 aqueous medium Substances 0.000 claims description 2
- 239000003054 catalyst Substances 0.000 claims description 2
- 239000012986 chain transfer agent Substances 0.000 claims description 2
- 229940011182 cobalt acetate Drugs 0.000 claims description 2
- QAHREYKOYSIQPH-UHFFFAOYSA-L cobalt(II) acetate Chemical compound [Co+2].CC([O-])=O.CC([O-])=O QAHREYKOYSIQPH-UHFFFAOYSA-L 0.000 claims description 2
- 238000007720 emulsion polymerization reaction Methods 0.000 claims description 2
- MGJURKDLIJVDEO-UHFFFAOYSA-N formaldehyde;hydrate Chemical compound O.O=C MGJURKDLIJVDEO-UHFFFAOYSA-N 0.000 claims description 2
- 230000000737 periodic effect Effects 0.000 claims description 2
- 150000002978 peroxides Chemical class 0.000 claims description 2
- 239000004014 plasticizer Substances 0.000 claims description 2
- XWGJFPHUCFXLBL-UHFFFAOYSA-M rongalite Chemical compound [Na+].OCS([O-])=O XWGJFPHUCFXLBL-UHFFFAOYSA-M 0.000 claims description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims 1
- 150000001242 acetic acid derivatives Chemical class 0.000 claims 1
- 239000007853 buffer solution Substances 0.000 claims 1
- 229940044175 cobalt sulfate Drugs 0.000 claims 1
- 229910000361 cobalt sulfate Inorganic materials 0.000 claims 1
- KTVIXTQDYHMGHF-UHFFFAOYSA-L cobalt(2+) sulfate Chemical compound [Co+2].[O-]S([O-])(=O)=O KTVIXTQDYHMGHF-UHFFFAOYSA-L 0.000 claims 1
- 125000002485 formyl group Chemical group [H]C(*)=O 0.000 claims 1
- 229910052700 potassium Inorganic materials 0.000 claims 1
- 239000011591 potassium Substances 0.000 claims 1
- 229910052708 sodium Inorganic materials 0.000 claims 1
- 239000011734 sodium Substances 0.000 claims 1
- 238000006243 chemical reaction Methods 0.000 description 15
- NBBJYMSMWIIQGU-UHFFFAOYSA-N Propionic aldehyde Chemical compound CCC=O NBBJYMSMWIIQGU-UHFFFAOYSA-N 0.000 description 8
- 239000002245 particle Substances 0.000 description 6
- 230000001070 adhesive effect Effects 0.000 description 4
- ZTQSAGDEMFDKMZ-UHFFFAOYSA-N butyric aldehyde Natural products CCCC=O ZTQSAGDEMFDKMZ-UHFFFAOYSA-N 0.000 description 4
- DOIRQSBPFJWKBE-UHFFFAOYSA-N dibutyl phthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 239000000853 adhesive Substances 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 2
- 238000007792 addition Methods 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 150000002148 esters Chemical class 0.000 description 2
- 238000005755 formation reaction Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 229920002554 vinyl polymer Polymers 0.000 description 2
- XXURNZLYJUXXCF-HJWRWDBZSA-N (z)-4-octan-3-yloxy-4-oxobut-2-enoic acid Chemical compound CCCCCC(CC)OC(=O)\C=C/C(O)=O XXURNZLYJUXXCF-HJWRWDBZSA-N 0.000 description 1
- IGFHQQFPSIBGKE-UHFFFAOYSA-N Nonylphenol Natural products CCCCCCCCCC1=CC=C(O)C=C1 IGFHQQFPSIBGKE-UHFFFAOYSA-N 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 238000004026 adhesive bonding Methods 0.000 description 1
- 150000001299 aldehydes Chemical group 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000000872 buffer Substances 0.000 description 1
- 150000001735 carboxylic acids Chemical class 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- HRKQOINLCJTGBK-UHFFFAOYSA-N dihydroxidosulfur Chemical compound OSO HRKQOINLCJTGBK-UHFFFAOYSA-N 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- GLVVKKSPKXTQRB-UHFFFAOYSA-N ethenyl dodecanoate Chemical compound CCCCCCCCCCCC(=O)OC=C GLVVKKSPKXTQRB-UHFFFAOYSA-N 0.000 description 1
- UIWXSTHGICQLQT-UHFFFAOYSA-N ethenyl propanoate Chemical compound CCC(=O)OC=C UIWXSTHGICQLQT-UHFFFAOYSA-N 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- ISXSFOPKZQZDAO-UHFFFAOYSA-N formaldehyde;sodium Chemical compound [Na].O=C ISXSFOPKZQZDAO-UHFFFAOYSA-N 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000005304 joining Methods 0.000 description 1
- SNQQPOLDUKLAAF-UHFFFAOYSA-N nonylphenol Chemical compound CCCCCCCCCC1=CC=CC=C1O SNQQPOLDUKLAAF-UHFFFAOYSA-N 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 229920000151 polyglycol Polymers 0.000 description 1
- 239000010695 polyglycol Substances 0.000 description 1
- 230000000379 polymerizing effect Effects 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 1
- 235000017557 sodium bicarbonate Nutrition 0.000 description 1
- VYGBQXDNOUHIBZ-UHFFFAOYSA-L sodium formaldehyde sulphoxylate Chemical compound [Na+].[Na+].O=C.[O-]S[O-] VYGBQXDNOUHIBZ-UHFFFAOYSA-L 0.000 description 1
- HFQQZARZPUDIFP-UHFFFAOYSA-M sodium;2-dodecylbenzenesulfonate Chemical compound [Na+].CCCCCCCCCCCCC1=CC=CC=C1S([O-])(=O)=O HFQQZARZPUDIFP-UHFFFAOYSA-M 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F18/00—Homopolymers 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
- C08F18/02—Esters of monocarboxylic acids
- C08F18/04—Vinyl esters
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/12—Polymerisation in non-solvents
- C08F2/16—Aqueous medium
- C08F2/22—Emulsion polymerisation
- C08F2/24—Emulsion polymerisation with the aid of emulsifying agents
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F20/00—Homopolymers and copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride, ester, amide, imide or nitrile thereof
- C08F20/02—Monocarboxylic acids having less than ten carbon atoms, Derivatives thereof
- C08F20/10—Esters
- C08F20/12—Esters of monohydric alcohols or phenols
Description
Foreliggende oppfinnelse vedrører en fremgangsmåte for fremstilling av polymerdispersjoner ved emulsjonspolymerisering av vinylestere, særlig vinylacetat, som eventuelt er tilsatt butylmaleinat, etylheksylmaleinat eller alkylakrylat med opptil 12 karbonatomer i alkylresten, i vandig medium i nærvær av en vannoppløselig redokskataly-sator og et buf f ers.ys tem, og eventuelt, i nærvær ,ay mykningsmidler og eventuelle vanlig anvendte tilsetningsmid- The present invention relates to a method for the production of polymer dispersions by emulsion polymerization of vinyl esters, in particular vinyl acetate, to which butyl maleinate, ethylhexyl maleinate or alkyl acrylate with up to 12 carbon atoms in the alkyl residue has been optionally added, in an aqueous medium in the presence of a water-soluble redox catalyst and a buffer. system, and possibly, in the presence of plasticizers and any commonly used additives
ler, og det særegne ved fremgangsmåten i henhold til oppfinnelsen er at polymeriseringen gjennomføres i to trinn, clay, and the distinctive feature of the method according to the invention is that the polymerization is carried out in two stages,
idet man i det første trinn ved temperatur 25-65°C kontinuerlig tilfører en vandig oksydasjonsblanding av vannløse-lige peroksyder og et bikarbonat og/eller acetat av et alkalimetall og et jordalkalimetall til en tilberedt blanding bestående av whereby in the first step at a temperature of 25-65°C, an aqueous oxidation mixture of water-soluble peroxides and a bicarbonate and/or acetate of an alkali metal and an alkaline earth metal is continuously added to a prepared mixture consisting of
a) 10 til 70 vekt% av den totalt anvendte monomerblanding, a) 10 to 70% by weight of the total monomer mixture used,
b) et stort overskudd i forhold til den støkiometriske mengde av et reduksjonssystem av natrium-formaldehyd-sulfoksylat og vann, og et acetat og/eller sulfat av. b) a large excess in relation to the stoichiometric amount of a reduction system of sodium-formaldehyde-sulfoxylate and water, and an acetate and/or sulfate of.
et element fra gruppe VIII i det periodiske system, an element from group VIII of the periodic table,
c) et vanlig beskyttelseskolloid, c) a common protective colloid,
d) et vanlig kapillaraktivt middel samt d) a common capillary active agent as well as
e) et vanlig kjedeoverføringsmiddel med aldehydfunksjon, hvoretter man i et annet trinn ved konstant temperatur e) a common chain transfer agent with an aldehyde function, after which in another step at constant temperature
ikke under 60°C kontinuerlig tilsetter ytterligere oksy-das jonsblanding og den resterende andel av monomermengden. not below 60°C continuously adds further oxidation ion mixture and the remaining proportion of the monomer quantity.
Disse og andre trekk ved oppfinnelsen fremgår av patent-kravene. These and other features of the invention appear in the patent claims.
Det er kjent å polymerisere vinylesteren alene eller sammen med de nærmere angitte monomerer ved en høy temperatur på 65-70°C, tilsvarende kokepunkttemperaturen for monomeren. It is known to polymerize the vinyl ester alone or together with the specified monomers at a high temperature of 65-70°C, corresponding to the boiling point temperature of the monomer.
Denne temperatur som til å begynne med ble oppnådd ved oppvarming med damp og høyere reaksjonstemperaturer, kunne anvendes ved å gjennomføre polymeriseringen under et lite overtrykk. This temperature, which was initially achieved by heating with steam and higher reaction temperatures, could be used by carrying out the polymerization under a slight excess pressure.
Det oppnås ved tidligere kjent teknikk korte reaksjonsperio-der men produktene har dårlig kvalitet, spesielt når de til-siktes brukt i klebemiddelindustrien. Short reaction periods are achieved by prior art, but the products are of poor quality, especially when they are intended to be used in the adhesives industry.
Det er nå overraskende funnet at det er mulig å overvinne ulempene med den kjente teknikk mens det oppnås produkter med høy kvalitet, ved å polymerisere ved lavere.temperaturer, It has now surprisingly been found that it is possible to overcome the disadvantages of the known technique while obtaining products of high quality, by polymerizing at lower temperatures,
i løpet av betraktelig kortere tidsrom og uten den initiale oppvarming av reaksjonskomponentene. during a considerably shorter period of time and without the initial heating of the reaction components.
Arbeidssekvens i samsvar med oppfinnelsen fører til dannelse Work sequence in accordance with the invention leads to formation
av 2 generasjoner av partikler, den første ved en lavere temperatur på fra 25-65°C med et høyt innhold av beskyttelseskolloid, og med en fordeling av partikkeldiameteren som er ganske bred, og den annen ved en høyere temperatur, idet denne temperatur dog er konstant og med en fordeling av par-tikkelstørreisene begrenset innen et snevere område. of 2 generations of particles, the first at a lower temperature of from 25-65°C with a high content of protective colloid, and with a distribution of the particle diameter that is quite broad, and the second at a higher temperature, this temperature being however constant and with a distribution of the particle size ices limited within a narrower area.
En slik heterogen karakter av partiklene er spesielt fordel-aktig ved fremstilling av klebemidler, hvorunder sammenføyningen av de stykker som skal forenes ved liming en viss del av polymer-partiklene må vandre i.nn j det indre av det porøse bæreelement. Such a heterogeneous nature of the particles is particularly advantageous in the production of adhesives, during which the joining of the pieces to be united by gluing a certain part of the polymer particles must move into the interior of the porous support element.
mens -de andre partikler forblir festet til utsiden/ slik at klebevirkningen av polymeren øker. -i while -the other particles remain attached to the outside/ so that the adhesive effect of the polymer increases. -in
En annet gunstig trekk ved fremgangsmåten i henhold til oppfinnelsen er at .-idet oppnås dispersjoner med en høyviskositets-verdi og en faktisk enestående konstans av ■viskositeten til tross for fortynning. Another favorable feature of the method according to the invention is that dispersions with a high viscosity value and an actually unique constancy of the viscosity despite dilution are obtained.
Det siste trekk er en av de mest interessante forutsetninger The last move is one of the most interesting assumptions
når det gjelder dispersjoner som skal anvendes for klebemidler og for vannbaserte malinger, .. sammen med de reologiske egen- , skaper og motstanden overfor skjærkrefter, som'også har en•høy verdi. when it comes to dispersions to be used for adhesives and for water-based paints, .. together with the rheological properties and the resistance to shear forces, which also have a high value.
Det er likeledes interessant å bemerke at ved passende variasjon av deler monomer i blandingen og i den.tilførte strøm, kan det oppnås emulsjoner med forskjellige-grader av polydispersivi tet og således forskjellige viskositetsnivåer, mens. de■beste tekno-logiske egenskaper og høy nytteevne bibeholdes.: Det er, også overraskende fastslått at ved å .anvendes- fremgangsmåten •.i henhold til :den foreliggende oppfinnelse oppnås det.' samtidig en vesentlig reduksjon i—tilsmussingen av. reaktoren; Fjernelsen av mulige spor,av s.korpedannelser foregår ved en--, enkel vasking med vann ved et lavt trykk. Andre spesielle for-deler som oppnås er økningen i effektiviteten av polymerisasjons-prosessen, som kvantitativt kan anslås til 40 - 50%. It is also interesting to note that by suitably varying the proportion of monomer in the mixture and in the supplied stream, emulsions with different degrees of polydispersity and thus different viscosity levels can be obtained, while. the ■best technological properties and high utility are retained.: It has also surprisingly been established that by using the method according to the present invention it is achieved. at the same time a significant reduction in—the soiling of. the reactor; The removal of possible traces of s.crust formations takes place by simple washing with water at a low pressure. Other special benefits that are achieved are the increase in the efficiency of the polymerization process, which can be quantitatively estimated at 40 - 50%.
Som angitt ovenfor kan fremgangsmåten i henhold; til oppfinnelsen anvendes for fremstilling av dispersjoner ved å gå ut fra vinyl-ester.e med eventuelle tilsetninger av de nærmere angitte estere av umettede syrer. Vinylacetat er angitt som en typisk vinyl-ester siden -det er denne som for tiden anvendes i de største mengder. As stated above, the procedure can according to; to the invention is used for the production of dispersions by starting from vinyl esters with any additions of the specified esters of unsaturated acids. Vinyl acetate is indicated as a typical vinyl ester since - it is this that is currently used in the largest quantities.
Andre vinylestere som kan anvendes er vinylpropionat, vinyl-laurat, og estere av umettede karboksylsyrer som har .gitt spesielt tilfredsstillende resultater er butylmaleinat,..etyl-héksylmaleinat, samt alkylakrylater hvori antallet av karbonatomer i alkylradikalet er lavere enn 12. Other vinyl esters that can be used are vinyl propionate, vinyl laurate, and esters of unsaturated carboxylic acids that have given particularly satisfactory results are butyl maleate, ethyl hexyl maleate, and alkyl acrylates in which the number of carbon atoms in the alkyl radical is lower than 12.
I det folgende gis noen eksempler på foretrukne utforelses-former for oppfinnelsen. In the following, some examples of preferred embodiments of the invention are given.
EKSEMPEL 1 - SAMMENLIGNING EXAMPLE 1 - COMPARISON
En 16 liters polymerisasjon reaktor av rustfritt stål, utstyrt med røreverk og tilbakeløpskondensator ble fylt med folgende sammensetning, referert til 100 deler monomerer. A 16 liter polymerization reactor of stainless steel, equipped with a stirrer and reflux condenser was filled with the following composition, referred to 100 parts of monomers.
Alle bestanddelene sammen med 20 deler vinyl-acetat innfores, oppvarmes til 68°C og polymeriseringen gjennomfores ved å tilfore det resterende vinylacetat i lopet av 4 timer ved en reaksjonstemperatur på 68-70°C. All the components together with 20 parts of vinyl acetate are introduced, heated to 68°C and the polymerization is carried out by adding the remaining vinyl acetate over the course of 4 hours at a reaction temperature of 68-70°C.
ANALYTISKE DATA ANALYTICAL DATA
EKSEMPEL 2 EXAMPLE 2
Til å begynne med innfores vann, polyvinyl-alkoholen som på forhånd var blitt opplost i vann, natrium-formaldehyd sulf-oksylatet, propionaldehydet, kobolt-acetatet og 40 deler av vinyl-acetatet. To begin with, water, the polyvinyl alcohol which had previously been dissolved in water, the sodium formaldehyde sulphoxylate, the propionaldehyde, the cobalt acetate and 40 parts of the vinyl acetate are introduced.
Deretter begynnes tilsetning av hydrogenperoksyd og bi.karbonat Then the addition of hydrogen peroxide and bicarbonate begins
i form av delmengder. in the form of partial amounts.
Ved 55°C innfores det resterende vinyl-acetat i lopet av 2 timer, idet reaksjonstemperaturen herunder holdes under 80°C. At 55°C, the remaining vinyl acetate is introduced over the course of 2 hours, the reaction temperature being kept below 80°C.
ANALYTISKE DATA ANALYTICAL DATA
EKSEMPEL 3 EXAMPLE 3
Fremgangsmåten er som i EKSEMPEL 2 med en reaksjonstemperatur som ikke overstiger 80°C. The procedure is as in EXAMPLE 2 with a reaction temperature that does not exceed 80°C.
ANALYTISKE DATA ANALYTICAL DATA
EKSEMPEL 4 EXAMPLE 4
Det innfores van^methylcellulose, natrium-dodecylbenzen-sulfonat og nonylfenol-polyglycol-eter , alle på forhånd-, opplost i vann, deretter propionaldehydet, natrium-formaldehyd, sulfoksylatet og 30 % av vinyl-acetatet og dibutylftalat. Van^methylcellulose, sodium dodecylbenzene sulphonate and nonylphenol polyglycol ether are introduced, all previously dissolved in water, then the propionaldehyde, sodium formaldehyde, the sulphoxylate and 30% of the vinyl acetate and dibutyl phthalate.
Hydrogenperoksyd og natrium-bikarbonat tilsettes så i delmengder etter at reaksjonen er kommet i gang, og det resterende vinyl-acetat og dibutylftalatet innfores, idet .reak-sjons temperaturen holdes ved omtrent 60°C. Hydrogen peroxide and sodium bicarbonate are then added in portions after the reaction has started, and the remaining vinyl acetate and dibutyl phthalate are introduced, the reaction temperature being kept at approximately 60°C.
ANALYTISKE DATA ANALYTICAL DATA
EKSEMPEL 5 EXAMPLE 5
Alle de ovennevnte bestandeler innfores, med unntakelse av hydrogenperoksydet og natrium-bikarbonatet, som tilsettes i delmengder i samsvar med temperaturnivået ved reaksjonen. All the above-mentioned ingredients are introduced, with the exception of the hydrogen peroxide and the sodium bicarbonate, which are added in partial amounts in accordance with the temperature level of the reaction.
Polymeriseringen gjennomfores ved en temperatur på 70°C som et maksimum. The polymerization is carried out at a temperature of 70°C as a maximum.
AN ALYTISKE DATA AN ALYTICAL DATA
EKSEMPEL 6 EXAMPLE 6
Fremgangsmåten er den samme som i EKSEMPEL 2, idet reaksjonstemperaturen ikke overstiger 75°C. The procedure is the same as in EXAMPLE 2, in that the reaction temperature does not exceed 75°C.
ANALYTISKE DATA ANALYTICAL DATA
EKSEMPEL 7 EXAMPLE 7
Fremgangsmåten er den samme som i EKSEMPEL 2. Reaksjonstemperaturen måles ved omtrent 70°C. The procedure is the same as in EXAMPLE 2. The reaction temperature is measured at approximately 70°C.
ANALYTISKE DATA ANALYTICAL DATA
EKSEMPEL 8 EXAMPLE 8
Fremgangsmåten er den samme som i EKSEMPEL 2, men 50 deler vinyl-acetat var blitt innfort til å begynne med og 50 deler tilfort kontinuerlig deretter. Reaksjonstemperaturen var 70°C The procedure is the same as in EXAMPLE 2, but 50 parts vinyl acetate had been introduced initially and 50 parts added continuously thereafter. The reaction temperature was 70°C
ANALYTISKE DATA ANALYTICAL DATA
EKSEMPEL 9 EXAMPLE 9
Fremgangsmåten er den samme som i EKSEMPEL 2, med en reaksjonstemperatur som ikke overstiger 70°C. The procedure is the same as in EXAMPLE 2, with a reaction temperature not exceeding 70°C.
ANALYTISKE DATA ANALYTICAL DATA
EKSEMPEL 10 EXAMPLE 10
Alle bestanddelene innfores sammen med 1/3 av vinyl-acetatet, vinyl-versatatet og propionaldehydet. Deretter begynner tilforsel av bikarbonat og hydrogenperoksyd. Med en temperatur på 60°C tilsettes det rest-., erende vinyl-versatat, vinyl-acetat og propionaldehyd til å begynne med og reaksjonstemperaturen måles slik at den ikke overstiger 80°C. Etter fullfort reaksjon og etter avkjoling tilsettes metanol og vann ( volum forhold 1:1)... All the components are introduced together with 1/3 of the vinyl acetate, the vinyl versatate and the propionaldehyde. Then the supply of bicarbonate and hydrogen peroxide begins. At a temperature of 60°C, the remaining vinyl versatate, vinyl acetate and propionaldehyde are initially added and the reaction temperature is measured so that it does not exceed 80°C. After the reaction is complete and after cooling, methanol and water are added (volume ratio 1:1)...
ANALYTISKE DATA ... ANALYTICAL DATA ...
Claims (3)
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| IT29601/76A IT1064497B (en) | 1976-11-22 | 1976-11-22 | PROCEDURE FOR THE PRODUCTION OF POLYMER OR COPOLYMER DISPERSIONS FROM VINYL ESTERS AND / OR CARBOXYLIC ACID ESTERS |
Publications (3)
| Publication Number | Publication Date |
|---|---|
| NO773948L NO773948L (en) | 1978-05-23 |
| NO150318B true NO150318B (en) | 1984-06-18 |
| NO150318C NO150318C (en) | 1984-09-26 |
Family
ID=11228080
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| NO773948A NO150318C (en) | 1976-11-22 | 1977-11-18 | PROCEDURE FOR PREPARING VINYLESTER POLYMER DISPERSIONS |
Country Status (19)
| Country | Link |
|---|---|
| AT (1) | AT363683B (en) |
| BE (1) | BE861061A (en) |
| CH (1) | CH629227A5 (en) |
| DE (1) | DE2752102C2 (en) |
| DK (1) | DK516177A (en) |
| EG (1) | EG12967A (en) |
| ES (1) | ES464654A1 (en) |
| FI (1) | FI63247C (en) |
| FR (1) | FR2392042A1 (en) |
| GB (1) | GB1567704A (en) |
| GR (1) | GR64097B (en) |
| IE (1) | IE45992B1 (en) |
| IT (1) | IT1064497B (en) |
| LU (1) | LU78551A1 (en) |
| NL (1) | NL7712817A (en) |
| NO (1) | NO150318C (en) |
| PT (1) | PT67300B (en) |
| SE (1) | SE432103B (en) |
| TR (1) | TR19944A (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE102007044788A1 (en) * | 2007-09-19 | 2009-04-02 | Wacker Chemie Ag | Preparation of vinyl acetate-vinyl ester copolymers with low content of high-boiling vinyl esters |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2998400A (en) * | 1958-05-15 | 1961-08-29 | Wyandotte Chemicals Corp | Floc-free polyvinyl acetate emulsions employing polyvinylmethyl ether copolymer as prtective colloid and process of preparation |
| FR1441940A (en) * | 1964-07-18 | 1966-06-10 | Hoechst Ag | Process for preparing aqueous dispersions of polymers of olefinic compounds |
-
1976
- 1976-11-22 IT IT29601/76A patent/IT1064497B/en active
-
1977
- 1977-11-02 GR GR54696A patent/GR64097B/en unknown
- 1977-11-11 FI FI773416A patent/FI63247C/en not_active IP Right Cessation
- 1977-11-16 EG EG647/77A patent/EG12967A/en active
- 1977-11-17 TR TR19944A patent/TR19944A/en unknown
- 1977-11-18 CH CH1415077A patent/CH629227A5/en not_active IP Right Cessation
- 1977-11-18 NO NO773948A patent/NO150318C/en unknown
- 1977-11-21 PT PT67300A patent/PT67300B/en unknown
- 1977-11-21 NL NL7712817A patent/NL7712817A/en not_active Application Discontinuation
- 1977-11-21 AT AT0832177A patent/AT363683B/en not_active IP Right Cessation
- 1977-11-21 GB GB48444/77A patent/GB1567704A/en not_active Expired
- 1977-11-21 DK DK516177A patent/DK516177A/en not_active Application Discontinuation
- 1977-11-21 FR FR7734945A patent/FR2392042A1/en active Granted
- 1977-11-21 LU LU78551A patent/LU78551A1/xx unknown
- 1977-11-21 SE SE7713139A patent/SE432103B/en unknown
- 1977-11-22 ES ES464654A patent/ES464654A1/en not_active Expired
- 1977-11-22 BE BE182819A patent/BE861061A/en not_active IP Right Cessation
- 1977-11-22 IE IE2367/77A patent/IE45992B1/en unknown
- 1977-11-22 DE DE2752102A patent/DE2752102C2/en not_active Expired
Also Published As
| Publication number | Publication date |
|---|---|
| IE45992L (en) | 1978-05-22 |
| SE7713139L (en) | 1978-05-23 |
| TR19944A (en) | 1980-05-08 |
| FI63247B (en) | 1983-01-31 |
| NL7712817A (en) | 1978-05-24 |
| GR64097B (en) | 1980-01-22 |
| NO773948L (en) | 1978-05-23 |
| EG12967A (en) | 1980-03-31 |
| FI773416A (en) | 1978-05-23 |
| GB1567704A (en) | 1980-05-21 |
| ATA832177A (en) | 1981-01-15 |
| DE2752102C2 (en) | 1982-11-04 |
| DK516177A (en) | 1978-05-23 |
| SE432103B (en) | 1984-03-19 |
| BE861061A (en) | 1978-05-22 |
| CH629227A5 (en) | 1982-04-15 |
| IT1064497B (en) | 1985-02-18 |
| FR2392042A1 (en) | 1978-12-22 |
| PT67300B (en) | 1979-04-20 |
| AT363683B (en) | 1981-08-25 |
| LU78551A1 (en) | 1978-04-13 |
| DE2752102A1 (en) | 1978-05-24 |
| FR2392042B1 (en) | 1981-10-23 |
| IE45992B1 (en) | 1983-01-26 |
| FI63247C (en) | 1983-05-10 |
| NO150318C (en) | 1984-09-26 |
| ES464654A1 (en) | 1978-09-01 |
| PT67300A (en) | 1977-12-01 |
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