CS268579B1 - Process for preparing terpolymer ethyl acrylate-methyl methacrylate-acrylonitrile water dispersion - Google Patents

Process for preparing terpolymer ethyl acrylate-methyl methacrylate-acrylonitrile water dispersion Download PDF

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CS268579B1
CS268579B1 CS879109A CS910987A CS268579B1 CS 268579 B1 CS268579 B1 CS 268579B1 CS 879109 A CS879109 A CS 879109A CS 910987 A CS910987 A CS 910987A CS 268579 B1 CS268579 B1 CS 268579B1
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ethyl acrylate
methyl methacrylate
weight
parts
acrylonitrile
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CS879109A
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Czech (cs)
Slovak (sk)
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CS910987A1 (en
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Ignac Rndr Csc Capek
Jaroslav Clen Korespond Barton
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Capek Ignac
Jaroslav Clen Korespond Barton
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Abstract

Účelom spósobu přípravy terpolymérovej etylakrylát-metylmetakrylát-akrylonitrilovej vodnej disperzie emulznou kopolymerizáciou je příprava stabilně) polyinérovej disperzie a zlepšenie regulácie polymerizačného procesu. Uvedený účel sa dosiihne tak, že sa pri přípravě terpolymérovej etylakrylát-metyl-metakry1át-akry1 onitri 1ovej vodnej disperzie použije 1,3 až 2,7 hmotnostných dielov nátrium-14-Lp-(l-nonyl)FenyloxyJ-3,6,9- -12-tetraoxatetradekanylsulfátu vzorca I. vztiahnuté na 100 hmotnostných dielov vody. Spčsob přípravy terpolymérovej ety 1 kry 1át-metylmeta-chémi i pri formulovaní nových postupov příprav nátěrových a impregnačných produktov.The purpose of the method for preparing a terpolymer ethyl acrylate-methyl methacrylate-acrylonitrile aqueous dispersion by emulsion copolymerization is to prepare a stable) polymer dispersion and to improve the control of the polymerization process. The stated purpose is achieved by using 1.3 to 2.7 parts by weight of sodium 14-Lp-(1-nonyl)phenyloxy-3,6,9- -12-tetraoxatetradecanyl sulfate of formula I. based on 100 parts by weight of water. The method for preparing a terpolymer ethyl acrylate-methyl methacrylate-acrylonitrile aqueous dispersion by emulsion copolymerization is also useful in formulating new processes for preparing coating and impregnation products.

Description

CS 268579 1)]CS 268579 1)]

Vynález ! i n týku spAsotiu prípinvy li; ι·ρο I ymi! rove j e ty I nk r y 1 á t-me t y lme Ink ty I á t-ak ty -lovej vodnej disperzie.The invention! i n t of spAsotion of adulteration li; ι · ρο I ymi! The present invention also relates to ink-containing water dispersions.

Polymerové vodné disperzíe připravené emulznou kopolymerlzáciou vinylových monomérovs rozdielnou rozpustnostou vo vodě mail Široké priemyselné použítie a boli predmetom mnohýchStudií c I· Čapek, 3. Bartoň: Makromoi. Chem. 1B6, 1297 (1985); 3. Guillot, Acta Polymerica 32, 593 (1901)3. Často sa připravovali polymerové disperzieakryiátových monomérov rozdielnej hydrofobnosti. Nevýhodou emuiznej kopolmerizácie týclitomonomérov je, ie takto vznikali polymerové la’texy s nízkou stabilitou, so zvýSenou možnos-lou koagulácie, nízkou viskozitou a s nízkým obsahom pevného polymčrovčho substrátu, Deláounevýhodou emuiznej kopolymerizácie akryiátových monomérov s rozdielnou rozpustnostou vovodě je, že tkto vznikali polymerové disperzie s nižšou stabilitou i pri vyšSích koncen-tráciach emulgátora (sodná soí kyseliny dodecylfenoxybenzéndisulfonovej, stearát sodný,alky 1 sulfonát sodný( Cl· Čapek, 3. Bartoň, E.Orolinová: Acta Polymerica 36, 107 (1985), 3. Guillot, Acta Polymerica 32, 593 (1981), 0. K. Švecov, T. D. Žukova, B. F. UstabSčikov, I. H. Kanevski, N. p. Petuchov, Acta Polymerica 32, 403 (1981)].Polymeric aqueous dispersions prepared by emulsion copolymerization of vinyl monomers with different solubility in water mail Wide industrial uses and have been the subject of many Studies c I · Čapek, 3. Bartoň: Makromoi. Chem. 1B6, 1297 (1985); 3. Guillot, Acta Polymerica 32, 593 (1901) 3. Polymer dispersion acrylate monomers of different hydrophobicity have often been prepared. The disadvantage of the emuizable copolymerization of tyclitomonomers is that they have a low stability polymer latex, with increased coagulation potential, low viscosity and low solid polymeric substrate content. lower stability even at higher emulsifier concentrations (sodium dodecylphenoxybenzene disulfonic acid, sodium stearate, sodium alkyl sulfonate (Cl · Capek, 3rd Barton, E.Orolinova: Acta Polymerica 36, 107 (1985), 3 Guillot, Acta Polymerica) 32, 593 (1981), 0. K. Svecov, TD Zhukov, BF UstabSchikov, IH Kanevski, N. Petuchov, Acta Polymerica 32, 403 (1981)].

Uvedené nevýhody v podstatnej miere odstraňuje spůsob přípravy terpolymerovej etylakrylát--mety lmetakrylát-akry lonitri lovej vodnej disperzie, ktorého podstata spočívá v tom, že sa při-dá 1,3 až 2,7 hmotnostných dielov nátrium-14-ζ p-(1-nonyl)fenyloxýj-3,6,9,12-tetraoxatetra-dekany1 sulfátu vzorca c9H19-^^H(0-CH2-CH2)5-0-S03Navztiahnuté na 100 hmotnostných dielov vody. výhodou navrhovaného spůsobu přípravy terpolymérového etyl-akrylát-metylmetakrylát-akry-r 1 onitrilového vodnej disperzie oproti doterajším spůsobom je že je vySšia stabilita kopoly-mérovej vodnej disperzie a rýchlost kopolymerizácie. Příklad 1The above disadvantages are substantially eliminated by the process for the preparation of terpolymer ethyl acrylate-methacrylate-acrylonitrile aqueous dispersion, which comprises adding 1.3 to 2.7 parts by weight of sodium-14-β- (1 -nonyl) phenyloxyl-3,6,9,12-tetraoxatetra-decane sulphate of the formula c9H19-N2H (O-CH2-CH2) 5-O-SO3, loaded on 100 parts by weight of water. The advantage of the proposed process for the preparation of the terpolymer ethyl acrylate-methyl methacrylate-acrylate onitrile aqueous dispersion is that there is greater stability of the copolymer water dispersion and the copolymerization rate. Example 1

Do trojhrdlej reakčnej banky objemu 1000 ml opatrenej miešadlom, spalným chladičom,prívodom pre dusík a zariadením pře kontinuálny odběr vzorky vodnej disperzie sa vdavkuje4 50 g destilovnej vody, 245 g etylakry 1 átu , 31,6 g metylmetakry1átu, 30,4 g akrylonitrilua 1,3 hmotnostných dielov ná t rium-14 - (j>-(1 -nony 1) f eny loxy2-3,6,9,12-te t raoxa te t radekany 1 -sulfátu (Etoxon AF-5). Po 30 minútovom miešaní pri 400 otáčkách za minutu a teplote 60°Csa přidá 0,6 persulfátu amonného. V priebehu polymerizácie sa odoberie každých 10 minut1 ml vodnej disperzie (na izoláciu polymeru k stanoveniu konverzie). Polymér sa izolujez vodnej disperzie tak, že sa disperzia skoaguluje v 50 ml metanolu okyselenom kyselinouoctovou na pH 2. Získaný polyfnér sa rozdrobí do zrnovej formy a premýva 100 ml vody a 100ml metanolu a nechá sa vysušit pri teplote 50 °C po dobu 5 dní. Z týchto získaných údajovsa vypočítává rýchlost polymerizácie v stacionárnom intervale ( I. Čapek, 3. Bartoň, E.Orolínová, Chemická Zvěsti 38, 803 (1984)). Po dopolymerizovaní monoméru finálna vodnádisperzia sa filtruje a získaný polymérový koagulát sa premýva 100 ml vody a 100 ml me-tanolu. Získaný koagulát sa suší po dobu 5 dní při teplote 50 °C. Rýchlost polymerizácieje 2,2 ΐ konverzie za minutu a získá sa 5 g polymerového koagulátu.50 g of distilled water, 245 g of ethyl acrylate, 31.6 g of methyl methacrylate, 30.4 g of acrylonitrile and 1 are introduced into a three-neck reaction flask equipped with a stirrer, a combustion condenser, a nitrogen inlet and a device for continuous sampling of the aqueous dispersion. 3 parts by weight of sodium-14 - (j - (1-nonylamino) -phenyl) -2,3,6,9,12-tetroxa-tetramate-1-sulfate (Etoxon AF-5). 0.6 Ammonium persulfate is added by stirring at 400 rpm and 60 ° C. Every 10 minutes, 1 ml of an aqueous dispersion (to isolate the polymer to determine the conversion) is taken during the polymerization, and the polymer is isolated from the aqueous dispersion so that the dispersion coagulates in 50 ml of methanol acidified to pH 2 with acetic acid. The obtained polyphene is crushed into a granular form and washed with 100 ml of water and 100 ml of methanol and allowed to dry at 50 ° C for 5 days. Interval Interval (I. Čapek, 3. Bartoň, E.Orolínová, Chemická Zvěsti 38, 803 (1984)). After the polymerization of the monomer, the final aqueous dispersion is filtered and the polymeric coagulum obtained is washed with 100 ml of water and 100 ml of methanol. The coagulum obtained is dried for 5 days at 50 ° C. The polymerization rate is 2.2 zie conversion per minute to obtain 5 g of polymer coagulum.

I Příklad 2Example 2

Postupuje sa ako v příklade 1, s tým rozdielom, že sa použijů 2 hmotnostné diely nátrium-- 1 4-Cp-(1-nony1)fenyloxý}-3,6,9,12-tetraoxatetradekanylsulfátu vztiahnuté na 100 hmotnostnýchdielov vody. Rýchlost polymerizácie je 2,6 \ konverzie za minutu a získá sa 2 g skoagulovanéhopolymeru.The procedure is as in Example 1, except that 2 parts by weight of sodium 1,4-Cp- (1-nonyl) phenyloxy} -3,6,9,12-tetraoxatetradecanyl sulfate per 100 parts by weight of water are used. The polymerization rate is 2.6 per minute per minute and 2 g of the coagulated polymer is obtained.

Claims (1)

CS 260579 Dl Příklad 3 Postupuje sa ako v příklade 1 s tým rozdielom, Je sa použije ako emulgátor 2,7hmotnostných dielov nátrium-lá-Cp-(l-nonyl )fenylox\PJ-J,6,9,12-tetraoxatctradekanyl-sulfátu vztiahnuté na 100 hmotnostných dielov vody. Rychlost polymerizácie je 3,1 \konverzic za minutu a nezíská sa židadny koagulát. Pře porovnanle účinku ná triům-14-£p-(1-nony 1) f eny loxy}-3,6,9 ,12-tetraoxa tetradekanylsulfátu s niektorým doteraz používaným emulgátorom, tj. na triům-17-oktadecén-1-sulfoná-tom, uvádzame nasledovný příklad Cl.Čapek, J. Bartoň, V. Svoboda, V. Novotný, L. Q. Tuan, Makromol. Chem . 1B8, 1723 ( 1987)3 : Příklad A Postupuje sa ako v příklade 1 s tým rozdielom, že sa použije ako emulgátor 3hmotnostně dlely nátrlum-17-oktadecěn-1-sulfonátu(Spolapon AOS), 240 g etylakrylátua 1Θ0 g metylmetakrylátu. Rýchlost polymerizácie je 3 t konverzie za minútu a získása 3 g koagulátu. Vynález může nájsi použitie v chemii přípravy polymerových disperzi! pri formulování nových typov stabilných latexových prípravkov. PRtDMCI VYNALEZU Spůsob přípravy terpolymerovej ety 1 akrylát-metylmetakrylát-akry1 onitri 1 ovej vodnejdisperzie emulznou kopolymerizaciou etylakrylátu, metylmetakrylátu a akrylonitrilu póso-bením persulfátu amonného, vyznačujúci sa, tým, že sa přidá 1,3 až 2,7 hinotnostných ná-trium-14Ep(l-nonyl)fenyloxyT-3,6,9,12-tctraoxatetradekanylsulfátu vzorcaEXAMPLE 3 The procedure is as in Example 1 except that it is used as an emulsifier of 2.7 parts by weight of sodium 1α-Cp- (1-nonyl) phenyloxypin-6,6,9,12-tetraoxatecradecanyl sulfate based on 100 parts by weight of water. The polymerization rate is 3.1 conversions per minute and no coagulum is obtained. For comparison, the effect of tri-14-β- (1-nonylamino) phenyloxy} -3,6,9, 12-tetraoxa tetradecanyl sulfate with some previously used emulsifier, i.e. tri-17-octadecene-1-sulfonic acid -tom, the following example of Cl.Kapek, J. Barton, V. Svoboda, V. Novotny, LQ Tuan, Makromol. Chem. 1B8, 1723 (1987) 3: Example A The procedure was as in Example 1 except that the 3-weight emulsion-17-octadecene-1-sulfonate (Spolapon AOS), 240 g of ethyl acrylate and 1-10 g of methyl methacrylate were used as emulsifiers. The polymerization rate is 3 t of conversion per minute to obtain 3 g of coagulum. The invention can find use in the chemistry of polymer dispersions! in formulating new types of stable latex formulations. EMBODIMENT A process for the preparation of terpolymer ethyl acrylate-methyl methacrylate-acrylonitrile water dispersion by emulsion copolymerization of ethyl acrylate, methyl methacrylate and acrylonitrile by coupling ammonium persulfate, characterized by the addition of 1.3 to 2.7 weight percent-14Ep (1-nonyl) phenyloxy-3,6,9,12-tetraoxatetradecanyl sulphate of formula vztiahnuté na 100 hmotnostných dielov vody.based on 100 parts by weight of water.
CS879109A 1987-12-12 1987-12-12 Process for preparing terpolymer ethyl acrylate-methyl methacrylate-acrylonitrile water dispersion CS268579B1 (en)

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