HRP20010009A2 - Self-crosslinking aqueous polystyrene-butadiene dispersions for consolidating bituminizable nonwovens and also consolidated nonwovens - Google Patents

Self-crosslinking aqueous polystyrene-butadiene dispersions for consolidating bituminizable nonwovens and also consolidated nonwovens Download PDF

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HRP20010009A2
HRP20010009A2 HR20010009A HRP20010009A HRP20010009A2 HR P20010009 A2 HRP20010009 A2 HR P20010009A2 HR 20010009 A HR20010009 A HR 20010009A HR P20010009 A HRP20010009 A HR P20010009A HR P20010009 A2 HRP20010009 A2 HR P20010009A2
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acid
parts
monomers
group
ingredient
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Gunther Mueller
Helmut Daum
Willibald Scheda
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Polymerlatex Gmbh & Co Kg
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Description

Izum se odnosi na samoumrežujuće disperzije polistirol-butadiena koje služe za ukrućivanje nosača slojeva na koje se može nanijeti bitumen, kao što su na primjer izolacijski krovni materijali s bitumenom, kao i vuneni materijali koji su očvrsnuti s disperzijom polistirol-butadiena.
EP-OS 0 438 284 opisuje vodene polimerne emulzije s niskim sadržajem slobodnog formaldehida, što se postiže uporabom sredstva za odstranjivanje formaldehida; kao sredstvo za odstranjivanje formaldehida koristi se N-metilolakrilamid. Spoj se koristi za umrežavanje polivinilacetata i disperzije vinilacetat-stirola.
WO 97/32930 opisuje vodenu disperziju čiji se sloj nanosi na tekstile od hidrofilnog poliuretana (PU) i kopolimerizata koji se sastoji od stirola, butadiena i ostalih monomera koji mogu kopolimerizirati s gore navedenim monomerom. Ove PU-disperzije koriste se za nanošenje na izolacijske krovne materijale.
DE-OS 40 29 733 opisuje povezane vunene materijale koji sadržavaju vezivu tvar u obliku disperzije, proizvodene pomoću polimerizacije konjugiranog diena, a,b-nezasićenih mono- ili dikarboksilnih kiselina, te olefinskog monomera s hidroksilnom skupinom.
US 4 125 663 obznanjuje postupak za proizvodnju povezanih vunenih materijala, pri čemu se polimerna disperzija dodaje kao umreživač kojeg čine smole melaimina i formaldehida.
Bituminirani krovni materijali proizvode se tako da se nosač sloja natopi i/ili premaže s bitumenom. Prije primijenjeni nosači sloja od kartona zamijenjeni su sa sirovim pustom, jutanom tkaninom, staklenom vunom, miješanom staklenom tkaninom, te prvenstveno poliesterskim vunenim pređama, kao i poliesterskim finim vunenim nitima zbog sve većih zahtjeva vezanih uz spomenuti prpizvod. Takvi vuneni materijali, koji su na primjer očvrsnuti s dispertijskim vezivima, moraju pri nanošenju bitumena i konačnoj primjeni imati slijedeća svojstva:
- neznatno rastezanje na temperaturama od 160 – 200 °C pri jakom razvlačenju, te visoku mehaničku čvrstoću
Povezujuća konstrukcija koje se sastoji od povezanog vunenog materijala smije se samo neznatno rastezati pri proizvodnim uvjetima impregniranja bitumena i/ili nanošenja sloja. 1 %-tno rastezanje ne smije se prekoračiti pri temperaturi od 160 – 200 °C i jakom razvlačenju zbog izrazite viskoznosti bitumena i velike brzine proizvodnje. Kod većih rastezanja pri hlađenju i razmotavanju izolacijskih krovnih materijala dolazi do fiksiranja naprezanja, koje nestaje pri ponovljenom zagrijavanju, na primjer uslijed zavarivanju šavova ili jakog sunčevog zračenja. To prouzrokuje pukotine u krovnoj strukturi. Smjer rastezanja može biti uzdužan, poprečan ili dijagonalan.
- dobro jamstvo za bitumen
- neznatnu osjetljivost na vodu, veliku gustoću vode
Kod nedovoljne hidrofobnosti vezanog vunenog materijala (materijal od niti, vezivno sredstvo) može doći do prodiranja vode na mjestima reza uslijed djelovanja pojedinačnih vlakana na principu fitilja. Ono dovodi do razdvajanja bitumena i povezanog vunenog materijala, ili pak do oštećenja uslijed smrzavanja.
- fleksibilnost i rastezljivost konstrukcije pri konačnoj primjeni
Zbog temperaturnih oscilacija kod konačne primjene (-40 °C do +80 °C) te različitog koeficijenta rastezanja različitih građevinskih materijala, cjelokupni izolacijski krovni materijal podliježe velikim oscilacijama dimenzije. Ako je cjelokupna konstrukcija kruta i nefleksibilna, nastaju fine pukotine, koje u kombinaciji s vlagom i hladnoćom dovode do uništenja izolacijskog krovnog materijala. Zbog toga izrazito je važno da na radnim temperaturama ne bude fleksibilan samo bitumen, već i podloga od povezanog vunenog materijala.
Sasvim iznenađujuće pronađeno je da spojevi stirolbutadiena sa samoumrežavajućim skupinama polimeriziraju, te su pogodni za impregniranje vunenih materijala. Tako dobiveni konačni proizvodi imaju na visokim temperaturama zahtjevanu postojanost dimenzije, te pokazuju neznatnu osjetljivost naspram vode. Mehanička svojstva na sobnoj temperaturi usporediva su sa standardnim sustavima.
Predmet izuma su samoumrežujuće vodene disperzije polistirol-butadiena koje služe za očvršćivanje vunenih materijal na koje se može nanijeti bitumen, a sastoje se od slijedećih monomernih sastojaka:
1) 20 do 55 dijelova, koji se odnose na suhu tvar disperzne faze, najmanje jednog konjugiranog diena,
2) 30 do 80 dijelova, koji se odnose na suhu tvar disperzne faze, najmanje jednog vinilaromatskog spoja sa sposobnošću kopolimerizacije,
3) 0,1 do 10 dijelova, koji se odnose na suhu tvar disperzne faze, najmanje jedne organske kiseline i/ili nijednog anhidrida sa sposobnošću polimerizacije,
4) 1 do 10 dijelova najmanje jednog umreživača,
5) 0 do 20 dijelova, koji se odnose na suhu tvar disperzne faze, najmanje jednog derivata α,β-nezasićene karboksilne kiseline.
Kao sastojak 1) posebno je pogodan 1,3-butadien. Mogu se također koristiti i drugi 1,3-dieni poput itoprena, klorizoprena ili 2,3-dimetilbutadina. Butadien je najpogodniji.
Najpogodniji sastojak 2) je stirol. Mogu se također koristiti ostali vinilaromati, kao što su na primjer metilstirol ili stirolkarboksilna kiselina.
Kao polimerizacijske organske karboksilne kiseline (sastojak 3) mogu se na primjer koristiti akrilna kiselina, metakrilna kiselina, itakonska kiselina, pojedinačno ili u smjesi. Također se mogu koristiti maleinska kiselina ili mravlja kiselina ili njihovi anhidridi. Najpogodnije za korištenje su akrilna i/ili metakrilna kiselina.
Kao sredstvo za umrežavanje (sastojak 4) koristi se prvenstveno akril- i metakrilamid. Za uporabu najpogodniji su slijedeći spojevi: N-metilolakrilamid, N-metoksimetilakrilamid, N-hidroksimetilakrilamid, N-metilolmetakrilamid, N-metoksimetilmetakrilamid ili N-hidroksilmetilmetakrilamid.
Kao derivati α,β-nezasićene karboksilne kiseline (sastojak 5) pogodni su slijedeći spojevi:. akril-, metakrilamid i/ili –nitril.
Mogu se također koristiti i smjese samoumrežavajućih disperzija za očvršćivanje vunenih materijala na koje se može nanijeti bitumen, opisane u nastavku.
Miješanjem “mekih” i “tvrdih” vrsta u primjeni mogu se dobiti različita željena svojstva vunenih materijala (kao na primjer savitljivost).
Na primjer tvrda SBR-vrsta ima slijedeći sastav: 60 % stirola, 28 % butadiena, 8 % akrilnitrila, 2 % kiseline i 4 % sredstva za umrežavanje; dok na primjer meka SBR-vrsta ima slijedeći sastav: 35 % stirola, 42 % butadiena, 10 % akrilnitrila, 7 % akrilamida, 2 % kiseline i 4 % sredstva za umrežavanje.
Općenito se odabire odnos od 7 : 3 do 0 : 10 mekog sastojka spram tvrdog sastojka.
Disperzije opisane u izumu za očvršćivanje vunenih materijala mogu sadržavati dodatne pomoćne i doknadne tvari, kao što su anionski emulgatori, neionski emulgatori, sredstva koja sprečavaju promjenu sastava, biocidi, sredstva za sprečavanje pjenjenja, pH-puferi, kompleksirajuće tvari.
Slijedeći predmet izuma predstavljaju očvrsnuti vuneni materijali, koji su očvrsnuti samoumrežujućom vodenom disperzijom polistirol-butadiena načinjene od slijedećih monomernih sastojaka:
1) 20 do 55 dijelova, koji se odnose na suhu tvar disperzne faze, najmanje jednog konjugiranog diena,
2) 30 do 80 dijelova, koji se odnose na suhu tvar disperzne faze, najmanje jednog vinilaromatskog spoja sa sposobnošću kopolimerizacije,
3) 0,1 do 10 dijelova, koji se odnose na suhu tvar disperzne faze, najmanje jedne organske kiseline i/ili njenog anhidrida sa sposobnošću polimerizacije,
4) 1 do 10 dijelova najmanje jednog umreživača,
5) 0 do 20 dijelova, koji se odnose na suhu tvar disperzne faze, najmanje jednog derivata a,b-nezasićene karboksilne kiseline.
Sa stajališta tehnike, kao vuneni materijali pogodni su svi poznati vuneni materijali, na primjer poput takvih materijala koji su načinjeni od stakla, polimera i prirodnih proizvoda, kao i smjesa, a posebno od sirovog pusta, jutane tkanine, staklene vune, miješane staklene tkanine, poliamida i poliestera. U okvirima izuma posebno pogodni za uporabu su poliesterske vunene pređe kao i poliesterske fine vunene niti. Uporabljeni vuneni materijali obrađuju se na način uobičajen za ovu namjenu, a to znači da se prišivaju odnosno termofiksiraju. Masa im je od 20 – 350 g/m2, odnosno 100 – 250 g/m2.
Sastojci 1) do 5) koji se koriste kao pomoćne i doknadne tvari iste su kao i za gore opisano.
Slijedeći primjeri trebaju pobliže opisati izum:
[image]
Što se tiče ostalih tvari važnih za polimerizaciju emulzije, kao što su inicijatori, emulgatori, tvari koje reguliraju molekulsku težinu i sredstva za sprečavanje promjene sastava, koriste se u proizvodnji one tvari koje sa stajališta tehnike odgovaraju vrsti i količini.
Primjer proizvodnog postupka
U kotao za polimerizaciju dodaju se demineralizirana voda, uobičajeni emulgatori, pomoćne tvari i monomeri.
Sadržaj se zagrije na oko 50 °C, nakon čega se doda sredstvo za stvaranje radikala. Temperatura se povisi (oko 90 °C), a polomerizacija se okonča tijekom 6 – 8 sati. Dobivena je nekoagulirana disperzija.
Potankosti proizvodnje opisane su u DE-OS 38 40 512 (Hüls AG), str. od 5 do 7, u Primjerima od 1 do 9 i od A do F.
Određivanje sadržaja krute tvari odvija se prema DIN 53 189.
Slijedećim disperzijama hotimice su okarakterizirane svojstva relevantna za tehničku primjenu:
[image]
Također su ispitivane smjese samoumrežujuć SBR-vrste. U primjeni miješanjem "meke" i "tvrde" vrste mogu se dobiti različita svojstava vunenih materijala (kao što je savitljivost).
Određivanje postojanosti dimenzije
Određivanje se odvija prema DIN 18192 (Točka 5.7).
Zbog karakterizacije predena vuna impregnira se pjenom slijedećeg sastava na Mathis-Foulard-u (pukotina: -10):
Vodena disperzija (50 %-tna): 250 g
Rohagit SL 215: 7,5 g (sredstvo za stvaranje pjene)
Rohagal 10 n: 1,0 g (stabilizator pjene)
VE-voda: 241,5 g
Sirova se vuna stegne prije impregniranja na temperaturi od 220 °C tijekom 5 minuta. Nakon impregniranja dolazi do sušenja i kondenzacije na temperaturi od 180 °C tijekom 10 minuta. Navedeni rezultati koji slijede predstavljaju srednju vrijednost tri pojedinačna određivanja.
Rohagit SL 215 je sredstvo za stvaranje pjene koje prodaje Röhm GbmH, a sastoji se od vodene otopine akrilatnog polimera.
Rohagal 10 n je stabilizator pjene kojeg prodaje Röhm GbmH, a sastoji se od neionskog tensida na osnovi masnog alkohola i polialkil etera.
[image]
Vuneni materijali koji su proizvedeni pomoću disperzija opisanih u izumu imaju vrlo malu tendenciju stezanja.
Predene vune, koje se impregniraju s navedenim tvarima u Primjeru 1 i Primjeru 2 ili sa smjesom koju čine oba, imaju usporedivu ili djelomično bolju postojanost dimenzije u odnosu na standardni sustav. Ovi proizvodi udovoljavaju zahtjevanim graničnim vrijednostima iz DIN-propisa. Ako se u izvedbi primjeni SBR bez samoumrežujuće skupine, tada rezultati nisu prihvatljivi prema DIN 18192. Takav sustav ne može se koristiti kao vuneni materijal.
Iz prakse je poznato da uslijed dodavanja smola melamin-formaldehida (MFH) ili sličnih spojeva, a u slučaju nedovoljne postojanost dimenzije, može doći do poboljšanja svojstava. Kao što je prikazano u slijedećem prikazu, to je također moguće i u slučaju poredbenog Primjera 3. No zahtijevane vrijednosti odnosno rezultati Primjera 1 i Primjera 2 nisu dosegnuti.
[image]
Pogodna melamin-formaldehid smola je npr. smola Cassurit MT (proizvođač: Clariant).
Određivanje visine penjanja
Za ispitivanje osjetljivosti na vodu i kapilarnost koriste se 3 cm široke trake povezanog i osušenog vunenog materijala koji se uranja vertikalno u vodenu kupelj. Dubina uranjanja iznosi 1 centimetar. Voda se može penjati samo vertikalno po povezanom vunenom materijalu. Određuje se visina penjanja u centimetrima nakon 24 sata.
[image]
Određivanje čvrstoće cijepanja povezanih vunenih materijala pomoću RT
Ispitivanje se izvodi uz oslanjanje na DIN EN ISO 527-1 i DIN EN ISO 527-3. Priprave se probni uzorci od vunenih materijala duljine 15 cm i širine 5 cm. Probni uzorci pohrane se u klimatiziranom prostoru na temperaturi od 23 °C te 50 %-tnoj relativnoj vlazi tijekom 24 sata, nakon čega se vrši karakterizacija pomoću Instron stroja za razvlačenje.
Ispitni parametri su:
Brzina rastezanja: 100 mm/min.
Debljina sloja vunenog materijala: 2 mm
Mjerno područje: 0 - 5000 N
Duljina napinjanja: 50 mm
Slijedi prikaz rezultata:
[image]
Postojanost na temperaturu
S obzirom da se povezani vuneni materijali prerađuju u vreloj bitumenskoj kupelji na temperaturi od 200 °C, kao što je gore opisano, interesantna je promjena mehaničkih svojstava vezanih uz temperaturne zahtjeve. Pošto polimeri stirol-butadiena i nakon polimerizacije sadržavaju dvostruke veze, nasuprot stirolakrilatima i čistim akrilatima, a mogu reagirati na visokim temperaturama s najrazličitijim spojevima, kao što su npr. radikali (kisik iz zraka), mora se pokloniti posebna pozornost promjeni svojstava vezanja koja se odnose na temperaturne zahtjeve.
Povezani vuneni materijali usijavaju se 30 minuta na 200 °C, nakon čega se vrši određivanje. U usporedbi sa standardnim sustavom stirolakrilata i čistih akrilata, vuneni materijali koji su tretirani sa SBR djelomično su obojani u intenzivnu smeđu boju. S obzirom da se kod konačne primjene vuneni materijal pokriva s dva sloja bitumena (gore i dolje), te se stoga ne vidi direktno, ovaj čisto optički nedostatak nije relevantan u primjeni. Pri ispitivanju mehaničkih svojstava (postojanost dimenzije) nakon usijavanja nije bilo moguće ustanoviti nikakvo pogoršanje koje se odnosi na rezultate.

Claims (14)

1. Samoumrežujuća vodena disperzija polistirol-butadiena, naznačena time da služi za očvršćivanje vunenih materijala na koje se može nanijeti bitumen, a sastoje se iz slijedećih monomernih sastojaka: 1) 20 do 55 dijelova, koji se odnose na suhu tvar disperzne faze, najmanje jednog konjugiranog diena, 2) 30 do 80 dijelova, koji se odnose na suhu tvar disperzne faze, najmanje jednog vinilaromatskog spoja sa sposobnošću kopolimerizacije, 3) 0,1 do 10 dijelova, koji se odnose na suhu tvar disperzne faze, najmanje jedne organske kiseline i/ili njenog anhidrida sa sposobnošću polimerizacije, 4) 1 do 10 dijelova najmanje jednog umreživača, 5) 0 do 20 dijelova, koji se odnose na suhu tvar disperzne faze, najmanje jednog derivata a,b-nezasićene karboksilne kiseline.
2. Disperzija prema zahtjevu 1, naznačena time da sastojak 1) čini najmanje jedan monomer odabran iz skupine monomera poput 1,3-butadiena, izoprena, klorizoprena i 2,3-dimetilbutadiena.
3. Disperzija prema najmanje jednom od zahtjeva 1-2, naznačena time da sastojak 2) čini najmanje jedan monomer odabran iz skupine monomera poput stirola, metilstirola i stirolkarboksilne kiseline.
4. Disperzija prema najmanje jednom od zahtjeva 1-3, naznačena time da sastojak 3) čini najmanje jedan monomer odabran iz skupine monomera akrilne kiseline, metakrilne kiseline, itakonske kiseline, maleinske kiseline i mravlje kiseline.
5. Disperzija prema najmanje jednom od zahtjeva 1-4, naznačena time da sastojak 4) čini najmanje jedan monomer odabran iz skupine monomera poput N-metilolakrilamida, N-metoksimetilakrilamida, N-hidroksimetilakrilamida, N-metilolmetakrilamida, N-metoksimetilmetakrilamida ili N-hidroksilmetilmetakrilamida.
6. Disperzija prema najmanje jednom od zahtjeva 1-5, naznačena time da sastojak 5) čini najmanje jedan monomer odabran iz skupine monomera poput akril-, metakrilamida i/ili –nitrila.
7. Očvrsnuti vuneni materijal, naznačen time da je ukrućen sa samoumrežujućom vodenom disperzijom polistirol-butadiena, koja se sastoji od slijedećih monomernih sastojaka: 1) 20 do 55 dijelova, koji se odnose na suhu tvar disperzne faze, najmanje jednog konjugiranog diena, 2) 30 do 80 dijelova, koji se odnose na suhu tvar disperzne faze, najmanje jednog vinilaromatskog spoja sa sposobnošću kopolimerizacije, 3) 0,1 do 10 dijelova, koji se odnose na suhu tvar disperzne faze, najmanje jedne organske kiseline i/ili njenog anhidrida sa sposobnošću polimerizacije, 4) 1 do 10 dijelova najmanje jednog umreživača, 5) 0 do 20 dijelova, koji se odnose na suhu tvar disperzne faze, najmanje jednog derivata a,b-nezasićene karboksilne kiseline.
8. Očvrsnuti vuneni materijal, naznačen time da disperzija sadržava sastojak 1) kojeg čini najmanje jedan monomer odabran iz skupine monomera poput 1,3-butadiena, izoprena, klorizoprena i 2,3-dimetilbutadiena.
9. Očvrsnuti vuneni materijal prema najmanje jednom od zahtjeva 7-8, naznačena time da sastojak 2) čini najmanje jedan monomer odabran iz skupine monomera poput stirola, metilstirola i stirolkarboksilne kiseline.
10. Očvrsnuti vuneni materijal prema najmanje jednom od zahtjeva 7-9, naznačena time da disperzija sadržava sastojak 3) kojeg čini najmanje jedan monomer odabran iz skupine monomera poput akrilne kiseline, metakrilne kiseline, itakonske kiseline, maleinske kiseline i mravlje kiseline.
11. Očvrsnuti vuneni materijal prema najmanje jednom od zahtjeva 7-10, naznačen time da disperzija sadržava sastojak 4) kojeg čini najmanje jedan monomer odabran iz skupine monomera poput N-metilolakrilamida, N-metoksimetilakrilamida, N-hidroksimetilakrilamida, N-metilolmetakrilamida, N-metoksimetilmetakrilamida ili N-hidroksilmetilmetakrilamida.
12. Očvrsnuti vuneni materijal prema najmanje jednom od zahtjeva 7-11, naznačen time da disperzija sadržava sastojak 5) kojeg čini najmanje jedan monomer odabran iz skupine monomera poput akril-, metakrilamida i/ili –nitrila.
13. Očvrsnuti vuneni materijal prema najmanje jednom od zahtjeva 7-12, naznačen time da se rabe vuneni materijali od stakla, polimera i prirodnih spojeva, kao i njihovih smjesa, a naročito od jutane tkanine, staklene vune, miješane staklene tkanine i poliestera.
14. Očvrsnuti vuneni materijal prema zahtjevu 13, naznačen time da se rabe vuneni materijali od poliesterske vunene pređe ili poliesterskih finih vunenih niti.
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