ࡱ> LG Ibjbjَ $PLq]222RRRR8< RALj(c c c ???????$B{D@2c A "c c c @5555c !R2?Fc ?55U;z?h"2?L`RRQ,X ?Usporedba klasi nih i novih ekoloakih sredstva za obradu protiv gu~vanja S. Bischof Vukuai, D. Katovi i I. Solja i Tekstilno-tehnoloaki fakultet Sveu iliata u Zagrebu, Zavod za tekstilnu kemiju i ispitivanje materijala Savska 16/5, 10 000 Zagreb, Hrvatska e-mail:  HYPERLINK mailto:sbischof@ttf.hr sbischof@ttf.hr  HYPERLINK mailto:dkatovic@ttf.hr dkatovic@ttf.hr  HYPERLINK mailto:isoljac@public.srce.hr isoljac@public.srce.hr Usporeena su klasi na sredstva za obradu celuloznih materijala protiv gu~vanja sa novim, ekoloaki povoljnim sredstvima koja ne sadr~e formaldehid. Primjenjenim neformaldehidnim sredstvima dimetilglioksalureom (DMGU) i polikarboksilnim kiselinama (PCA), koji se meusobno potpuno razlikuju po mehanizmu reakcije, dobiveni su podjednako dobri efekti obrade protiv gu~vanja kao i sa klasi nim sredstvima na bazi N-metilolnih spojeva. Primjenom kombinacije sredstava DMDHEU/DMGU postignuto je znatno smanjenje formaldehida uz istovremeno ispunjenje ekonomskih zahtjeva. Poboljaanje mehani kih svojstava djelomi no je postignuto primjenom eterificirane DMDHEU, a u znatnijoj je mjeri postignuto primjenom neformaldehidnih sredstava. Na promjene nijanse obojenja prema naaim ispitivanjima najmanji utjecaj imaju PCA, dok je utjecaj derivata DMDHEU i DMGU podjedanak kod svih primjenjenih reaktivnih bojila. Klju ne rije i: obrada protiv gu~vanja, slobodni formaldehid, DMDHEU, DMGU, PCA Uvod / Introduction Visoko oplemenjivanje celuloznih materijala nastalo je kao nu~na posljedica ~elje za poboljaanjem svojstava prirodnih celuloznih materijala. Ovom obradom se celuloznim materijalima daju neka nova svojstva koja ona do tada nisu imala, no usporedno mo~e doi i do nekih negativnih efekata obrade (Tablica 1). Od 80-tih godina do danas naj eae primjenjivano sredstvo za obradu protiv gu~vanja je 1,3 dimetilol 4,5 dihidroksietilen urea (DMDHEU) koja se primjenjuje uz katalizator MgCl2 (Tablica 2). Najvei problem koji se javlja kod ove vrste N-metilolnih spojeva za obradu protiv gu~vanja je problem oslobaanja formaldehida, do kojeg naro ito dolazi na viaim temperaturama termi kih obrada. To oslobaanje formaldehida uzrokovalo je velike poteakoe zbog bojazni da je formaldehid toksi an i kancerogen, a dokazano je i njegovo alergijsko dermatiti no djelovanje1. Zbog toga je otpuatanje formaldehida u otpadni zrak nakon procesa termokondenzacije ograni eno na 20 ppm u nekim Europskim zemljama. Takoer je koli ina dozvoljenog slobodnog formaldehida u tekstilijama strogo ograni ena i ovisna o namjeni samog proizvoda (Tablica 3). Ukoliko je proizvod namjenjen za dje ju odjeu postavljaju se vrlo strogi zahtjevi da takav proizvod ne smije uope sadr~avati formaldehid. Postavljeni zahtjevi su vrlo esto pretjerani, pa je teako razlu iti da li su oni zaista postavljeni iz ekoloakih razloga ili ipak zbog ekonomskih razloga zatvaranja tr~iata. Tekstilni materijali moraju ispunjavati navedene ko-tex zahtjeve u svim Europskim zemljama. Ova oznaka garantira da korisnici tekstilnih proizvoda nee biti izlo~eni iritacijama ko~e, niti penetraciji atetnih supstanci sa tekstilnog materijala za vrijeme koriatenja proizvoda. U praksi se vrlo teako posti~e da proizvod uope ne sadr~i formaldehid, jer se utvrdilo da i neobraene tekstilije od pamuka i PES/pamuka mogu imati do 12 ppm slobodnog formaldehida. Formaldehid je osim toga svuda prisutan u naaoj okolini i normalan je produkt izmjene tvari. On se nalazi i u okolnom zraku, no fotokemijskim reakcijama se brzo dalje oksidira do uglji nog dioksida. Zbog navedene ekoloake problematike razvoj proizvoda za obradu protiv gu~vanja tekao je s nastojanjem da se koli ina slobodnog formaldehida smanji (sredstva siromaana formaldehidom) ili potpuno ukloni (sredstva bez formaldehida). Smanjenje otpuatanja formaldehida postignuto je na razli ite na ine: naknadnim pranjem nakon termokondenzacije dodatkom hvata a formaldehida (npr. karbohidrazida) dodatkom 10  30 % uree modifikacijom DMDHEU sa alkoholima  eterificiranje modifikacijom DMDHEU sa dietilenglikolom ili 2,3 propandiolom2. Ovim na inima koli ina otpuatenog formaldehida uspjela se znatno smanjiti, ali da bi se ispunili strogi zahtjevi da formaldehida uope ne bude na materijalu potrebno je primjeniti sredstva koja ne sadr~e formaldehid, tzv. neformaldehidna sredstva. Tijekom 90-tih godina po ela su intenzivna istra~ivanja za pronala~enjem zamjene za N-metilirane spojeve. Jedan od takvih spojeva je 1,3 dimetil 4,5 dihidroksietilen urea (DMeDHEU). Zbog mogunosti zamjene ovog spoja sa klasi nim DMDHEU eae se primjenjuje naziv: dimetil glioksalurea (DMGU). Ovo sredstvo je zbog smanjene reaktivnosti (hidroksilne skupine su zamjenjene metilnim) potrebno primjenjivati u znatno viaim koli inama, ato je vrlo negativno s ekonomskog aspekta, a obraeni materijali imali su i neugodan miris. Djelotvornost glioksala mo~e se zna ajno poboljaati dodatkom glikola koji povoljno djeluje na reakciju umre~avanja, kao i na strukturu nastalih umre~enja. Osim toga glikol uveliko smanjuje po~uenje do kojeg mo~e doi kad se celulozni materijal obrauje glioksalom u prisustvu kiselih katalizatora3. Najnovija istra~ivanja uklju uju i ispitivanja mogunosti primjene dialdehida kao sredstva za obradu protiv gu~vanja. U usporedbi sa DMGU ovom obradom su dobiveni bolji efekti obrade, prvenstveno bolji kutevi oporavka i manje promjene stupnja bjeline obraenog materijala. U usporedbi sa eterificiranom DMDHEU, kutevi oporavka su neato ni~i, ali je smanjen gubitak vrstoe koji je bio velik problem kod klasi ne obrade protiv gu~vanja4. Slijedea mogunost primjene neformaldehidnih spojeva ukazala se pojavom polikarboksilnih kiselina. Iako su se one prvi put po ele istra~ivati ve u 60-tim godinama zbog neodgovarajuih katalizatora postignuti efekti obrade nisu bili zadovoljavajui. Tek primjenom alkalno metalnih soli kiseline koja sadr~i fosfor postignuti su zadovoljavajui efekti obrade, najbolji primjenom natrijevog dihidrogen hipofosfita. Ova alternativna metoda razvijena je u laboratorijima U.S. Department of Agriculture, Southern Regional Research Center5. Polikarboksilne kiseline umre~avaju se s celulozom potpuno druga ijim mehanizmom reakcije, jer dok je kod klasi nih N-metilolnih sredstava mehanizam reakcije eterifikacija, ovdje je prisutna esterifikacija6. Mehanizam same reakcije dugo nije bio sa sigurnoau utvren, no pokazala se ispravnost pretpostavke da se reakcija odvija u dva stupnja, pri emu u prvom stupnju nastaje cikli ki anhidrid, a u slijedeem stupnju reaktivni anhidrid reagira sa celuloznim hidroksilnim skupinama7. Dosada su u praksu uvedena sredstva na bazi 1,2,3,4-butantetrakarboksilne kiseline (BTCA), kao i polimerno sredstvo bazirano na maleinskoj i akrilnoj kiselini, te vinil alkoholu. U usporedbi sa klasi nom DMDHEU ova sredstva su pokazala zna ajna poboljaanja mehani kih karakteristika  prvenstveno poboljaanje vrstoe i otpornosti materijala na habanje. Glavni nedostatak BTCA je visoka cijena proizvoda, no kineski proizvoa i su uspjeano rijeaili i ovaj problem. Uvoenje jeftinijih polimernih sredstava na bazi maleinske i akrilne kiseline predlo~io je prof. C.Q. Yang sa University of Georgia, koji predmijeva njihovo brzo uvoenje u airu praksu8. U radu su efekti obrade postignuti primjenom novih neformaldehidnih sredstava, kao i sredstava sa smanjenom koli inom formaldehida, usporeeni sa efektima dobivenim primjenom klasi nog N  metilolnog sredstva DMDHEU. Primjenjena je i jedna receptura koja kombinira neformaldehidno sredstvo (DMGU) i sredstvo sa smanjenom koli inom formaldehida (eterificirana DMDHEU) u svrhu zadovoljenja ekonomskih zahtjeva, uz zadr~avanje dobrih efekata obrade protiv gu~vanja9. Nadalje se ~eljelo pokazati da polikarboksilne kiseline, kao nova ekoloaki povoljnija sredstva, imaju va~nu ulogu u zamjeni klasi nih, neekoloakih sredstava za obradu protiv gu~vanja. Najva~niju ulogu kod odabira neformaldehidnih sredstava ima ekonomski faktor, te je u tu svrhu izabrana limunska kiselina koja zahtjeve sa ekonomskog i ekoloakog aspekta u potpunosti zadovoljava10. Neato loaije efekte obrade postignute primjenom limunske kiseline, nastojalo se u prijaanjim radovima11 poboljaati primjenom mikrovalne tehnologije. Pokazalo se da ovaj na in termi ke obrade znatno utje e na poboljaanje efekata, prvenstveno kuteva oporavka, te omoguuje primjenu ove manje reaktivne polikarboksilne kiseline. Eksperimentalni dio / Experimental Materijal / Vrsta obrade / Material / Finishing U radu su primjenjene (odakrobljena, iskuhana, kemijski bijeljena i mercerizirana) pamu na tkanina - povrainske mase 105 g/m2, te viskozna tkanina  povrainske mase 120 g/m2. Na viskoznom materijalu praen je utjecaj apreturnih sredstava na promjene obojenja, te je u tu svrhu materijal bojadisan na laboratorijskom aparatu "Turbomat 1000"Ahiba, reaktivnim bojilima sa vinil sulfonskom (VS) reaktivnom grupom. Primjenjena su slijedea Bezaktiv bojila: Yellow V-7GL, Brillant Red V-B, Brillant Blue V-R, Black V-GRA. Bojadisanje je provedeno sa 0,2 % bojila, uz omjer kupelji 1:15 i ukupno vrijeme obrade 2 sata, prema propisima proizvoa a. Standardni aditivi su koriateni u procesu bojadisanja: A: Meropan NX (1,0-2,0 g/l), Biavin 109 (0,3 g/l), bojilo 0,2 4 %; B: NaCl (30-80 g/l); C: Na2CO3 (5,0 g/l); D: NaOH 38 B (0,5-3 ml/l); E: acetatna kiselina (1,0 ml/l); F: Cotoblanc NSR (0,3 g/l). Sva bojila i dodaci za bojadisanje su proizvedeni u tt. Bezema AG, Montlingen, vicarska. Nakon procesa bojadisanja materijal je apretiran sa sredstvima za obradu protiv gu~vanja navedenim u tablici 4, a njihove formule su prikazane na slici 1. Uzorci su fulardirani na laboratorijskom ureaju uz efekt cijeenja oko 100% i kontinuirano suaeni na rasteznom suaioniku (Benz, `vicarska) na 110( C u vremenu od 2 minute. Termi ka obrada je provedena na istom ureaju za sredstva na bazi DMDHEU u vremenu od T= 150(C, t= 5 min., a za sredstva na bazi PCA T=180(C, t = 90 s. Mjerne metode / Methods CIE stupanj bjeline (WI) i stupanj po~uenja (YI) obraenih materijala mjereni su na refleksijskom spektrofotometru Datacolor 3890 (`vicarska) sa D65/10 rasvjetom. Kutevi oporavka (WRA) su mjereni prema metodi: ISO 2313 (DIN 53891), prekidna vrstoa je mjerena u smjeru osnove i potke prema metodi: ISO 13934-1 (DIN 53837), a otpornost na habanje je mjerena po metodi Martindale prema: ISO 12947-2 na Mesdan aparatu (Italija). Slobodni formaldehid je odreivan prema ISO 14184 - 1 metodi. Rezultati i diskusija / Results and discussion U radu je ispitan sadr~aj slobodnog formaldehida na pamu nom i viskoznom materijalu u vremenskom periodu od mjesec dana (Slika 2.). Primjeeno je da je koli ina slobodnog formaldehida zna ajno viaa na viskoznim materijalima nego na pamu nim. Takoer je dobivena primjetno viaa koli ina primjenom katalizatora Zn(NO3)2 nego MgCl2 , ato je naro ito uo ljivo na viskoznoj tkanini. Izborom i kombinacijom recepture koja sadr~i sredstvo bez formaldehida i sredstvo siromaano formaldehidom (DMGU/DMDHEU) nastojali smo dobiti takve rezultate koji bi mogli zadovoljiti postro~ene zahtjeve kupaca i postojeih standarda, bez potrebe naknadnog pranja koje znatno poskupljuje proizvodni proces. U odnosu na sredstva s niskom koli inom formaldehida postignuto je smanjenje na pamu nom materijalu 20-50%, ime dolazimo do granice oko ili ispod 75 ppm (Tablica 3), ato ispunjava zahtjev za dozvoljenom koli inom slobodnog formaldehida za odjeu blizu ko~e. Rezultati ukazuju na mogunost koriatenja ove recepture u praksi, ime bi se u veini slu ajeva izbjeglo naknadno pranje i suaenje. Dobiveni kutevi oporavka primjenom kombinacije ovih sredstava su podjednaki onim, dobivenim uz sredstva sa smanjenom koli inom slobodnog formaldehida. Kombinacija ovih apretura mogla bi zadovoljiti i stroge zahtjeve za odjeu za bebe (< 20 ppm), ako bi se materijal podvrgnuo naknadnom pranju. Ve nakon prvog pranja koli ina slobodnog formaldehida se smanjila na svega 5 ppm. Visoki rezultati bjeline dobiveni na viskoznom materijalu uzrokovani su dodatkom opti kih bjelila u apreturnu kupelj (Tablica 5). Rezultati mjerenja stupnja bjeline kemijski bijeljenih uzoraka pokazali su vei utjecaj apreturnih sredstava na viskozni materijal, nego na pamu ni. Ta problematika je naro ito izra~ena kod limunske kiseline koja je najosjetljivija na visoke termokondenzacijske temperature, jer one uzrokuju njen raspad na nezasiene kiseline (akonitnu, itakonsku i citrakonsku) ije konjugirane dvostruke veze uzrokuju po~uenje. Ranije provedena ispitivanja su pokazala da primjena Na-hipofosfita, kao najefikasnijeg katalizatora za obradu s PCA, u dovoljnim koli inama djelomi no smanjuje po~uenje materijala. Openito, primjenom polikarboksilnih kiselina dobivene su ni~e vrijednosti stupnja bjeline nego kod klasi nih N-metilolnih spojeva. Uz sredstvo na bazi DMGU postignuti su zadovoljavajui rezultati bjeline, te neato bolji primjenom kombinacije apreturnih sredstava DMGU/DMDHEU koja je na viskozi dala najbolje efekte. No, najbolji rezultati stupnja bjeline postignuti su ipak klasi nim sredstvom na bazi DMDHEU. Na pamu nom materijalu praen je utjecaj pojedinih apretura protiv gu~vanja na njegova fizikalna svojstva: kuteve oporavka, prekidnu vrstou i otpornost na habanje (Tablica 6). Klasi na sredstva za obradu protiv gu~vanja, iako daju visoke efekte obrade protiv gu~vanja (iskazane primarno kutevima gu~vanja), imaju veliki nedostatak smanjenje mehani kih svojstava materijala  zadr~ane prekidne sile i otpornosti na gu~vanje. Primjenom sredstava sa smanjenom koli inom formaldehida (eterificirana DMDHEU) postignuto je poboljaanje otpornosti na habanje, no do zna ajnijeg poboljaanja rezultata doalo je primjenom neformaldehidnih spojeva. Usporedbom rezultata kuteva oporavka limunske kiseline i BTCA vidljivo je da CA pokazuje znatno manju reaktivnost u odnosu na tetrakarboksilnu kiselinu. Ni~a reaktivnost CA tuma i se razlikom ve u prvoj fazi reakcije, jer primjenom ove trikarboksilne kiseline dolazi do nastajanja manjeg broja anhidrida nego primjenom BTCA, te je i broj esterskih veza koje nastaju u drugoj fazi reakcije manji. S obzirom da je za postizanje dobrih efekata obrade potrebno ostvariti umre~avanje, odnosno dvostrano ili viaestruko povezivanje sa hidroksilnim skupinama celuloznog lanca, efekti dobiveni limunskom kiselinom su slabiji. U svrhu poboljaanja efekata obrade provoena su i ispitivanja primjenom kombinacije ovih apreturnih sredstava, jer i mala koli ina BTCA djeluje kao ekstender na CA i zna ajno poboljaava njene efekte12. Usporedbom rezultata kuteva oporavka vidljivo je da su efekti postignuti sa neformaldehidnim spojevima (BTCA i DMGU) podjednako dobri kao oni postignuti klasi nim spojevima na bazi DMDHEU. Dodatna prednost PCA je da ona prema naaim ispitivanjima znatno manje utje u na promjenu nijanse obojenja reaktivnih bojila, nego ato utje u derivati DMDHEU ili DMGU (Slika 3.). Uz veinu primjenjenih bojila dobivene su podjednake promjene obojenja (izra~ene kao CIELab dE) primjenom DMGU i DMDHEU spojeva. Nadalje, u svim slu ajevima primjene reaktivnih vinilsulfonskih bojila (osim kod ~utog tona) dobivene su vee promjene obojenja primjenom katalizatora Zn(NO3)2. Potvreni su ranije naeni rezultati da do najveih promjena dolazi u zasienosti. Prema podacima iz literature, u slu aju primjene sredstava za obradu protiv gu~vanja na bazi PCA na promjenu obojenja najvei utjecaj ima katalizator Na-hipofosfit koji je jaki reducens13. Te promjene su najja e izra~ene kod sumpornih bojila, ali mogu se pojaviti i kod nekih reaktivnih, kao i reduktivnih bojila, te je bilo potrebno ispitati njihov utjecaj zbog eventualnog korigiranja same recepture za bojadisanje. Zaklju ak / Conclusion Kombiniranom recepturom DMGU/DMDHEU dobiveni su rezultati koji zadovoljavaju stroge zahtjeve za dozvoljenu koli inu slobodnog formaldehida na materijalu za odjeu blizu ko~e. Podvrgavanjem obraenog materijala naknadnom pranju koli ina slobodnog formaldehida je znatno smanjena, te zadovoljava i najstro~e zahtjeve za odjeu za bebe. Primjenom sredstava sa smanjenom koli inom formaldehida postignuto je poboljaanje mehani kih svojstava materijala, a daljnje poboljaanje je postignuto primjenom neformaldehidnih spojeva. Pritom su efekti obrade, izra~eni prvenstveno kao kutevi oporavka, podjednako dobri kod neformaldehidnih sredstava (DMGU i BTCA) kao i kod klasi nih DMDHEU sredstava. Limunskom kiselinom su dobiveni ni~i efekti obrade, ato se objaanjava manjim brojem veza koje se mogu uspostaviti izmeu anhidrida trikarboksilne limunske kiseline i hidroksilnih grupa celuloze. Dodatna prednost ekoloaki povoljnih PCA je da ona znatno manje utje u na promjene obojenja nego klasi na sredstva na bazi DMDHEU. Zbog navedenih prednosti budunost se predvia u primjeni pojedinih polikarboksilnih kiselina kod kojih je mogue ispuniti kako ekoloake, tako i ekonomske zahtjeve uz zadr~avanje dobrih efekata obrade. Literatura / References I. Solja i, D. Katovi, Tekstil 41(1992) 11, 545-554. I. Holme, Text Hor. 17 (1997) 2/3,17-24. C.M. Welch, G.M. Danna, Text. Res. J. 52 (1982) 149-157. C.Q. Yang, W. Wei, Text. Res. J., 70 (2000) 3, 230-236. C.M. Welch, Textile Res. J. 70 (1988) 8, 480-486. S. Bischof Vukuai, D. Katovi, I. Solja i, Tekstil 48 (1999) 11, 549-561. D. Katovi, S. Bischof Vukuai, G. `tefani, Tekstil 49 (2000) 10, 551-554. C.Q. Yang, Am. Dyest. Rep. 31 (1999) 5, 13-16. S. Bischof Vukuai, I. Solja i, D. Katovi, American Dyestuff Reporter 85 (1996) 5, 21-27. S. Bischof Vukuai, D. Katovi, Tekstil 51 (2002) 7, 325-330. D. Katovi, S. Bischof Vukuai, AATCC Rewiev 2 (2002) 4, 39-42. B. A. Kottes Andrews, Text. Chem. Color. 22 (1990) 9, 63-67. H. Choi H., R.D. Goodin, T.D. Pratt, Am. Dyest. Rep. 26 (1994) 2, 38-51. POPIS TABLICA Tablica 1 - Postignuti efekti obrade protiv gu~vanja Table 1 - Effects of Durable Press (DP) Finishing NEGATIVNE STRANE OBRADE NEGATIVE ASPECTSPOZITIVNE STRANE OBRADE POSITIVE ASPECTS- smanjenje vrstoe - decrease of mechanical strength -bolja dimenzionalna stabilnost - better dimensional stability - smanjenje bjeline - decrease of whiteness degree - bolje zadr~avanje oblika - better shape retention- smanjenje sorpcije - decrease of sorption- manje gu~vanje - less crease formation - mogua promjena nijanse - possible shade changes- lakae gla anje - easier care - mekoa i glatkoa - improved softness and smoothness - manja sklonost pilingu - reduction of peeling - bolja postojanost obojenja - better colour fastness Tablica 2 - Povijesni razvoj sredstava za obradu protiv gu~vanja Table 2 - Development of DP finishing agents Godina YearSredstvo za obradu protiv gu~vanja Reactant for DP finishing1928-1930Termokondenzacijski spojevi: -pretkondenzati urea-formaldehidnih smola - precured urea-formaldehyde resins 1930-derivati melaminskih smola - derivatives of melamine resins 1945Reaktivni spojevi: - dihidroksimetilen urea (DMEU) - dihydroxymethylene urea 1948- derivati etilirane uree - derivatives of ethylated urea 1954- dimetilol dihidroksi etilen urea (DMDHEU) - dimethyloldihydroxyethylene urea 1958-1959- derivati dihidroksietilenuree (DHEU) - derivatives of dihydroxyethyleneurea 1978-1980Dimetilglioksal urea (DMGU) Dimethylglioxalurea 1988Polikarboksilne kiseline (PCA) Polycarboxylic acids Tablica 3 - Grani ne vrijednosti za formaldehid (ppm) prema ko-Tex Standardu 100 Table 3 - Allowed values of free formaldehyde content (ppm) according to ko-Tex Standard ko-Tex Standard 100101102103104105106Ispitivanja InvestigationsTekstilno ploani proizvodi TextilesPomoni materijali za odjeu AccessoriesOdjea ClothesTekstilno ploani proizvodi za bebe Textiles for babiesPomoni materijali za odjeu za bebe Accessories for babies Odjea za bebe Baby clothesFormaldehid slobodan i dijelom otcjepljiv Free formaldehyde  20 20 20Odjea udaljena od ko~e Products without direct skin contact  300 300 300Odjea blizu ko~e Products in direct skin contact 75  75 75 Tablica 4 - Primjenjena sredstva Table 4 - Applied reactants Apretura Bath  Reaktant Reactant (g/l) Katalizator Catalyst (g/l) Tenzid Surfactant (g/l)1 DMDHEU120MgCl216Neionski Nonionic12 AEterificirana DMDHEU 120na bazi MgCl2 based on MgCl2 16Neionski12 BEterificirana DMDHEU 120na bazi Zn(NO3)216Neionski13 ADMGU 180na bazi MgCl230Neionski13 BDMGU180 na bazi Zn(NO3)2 30Neionski14 ADMGU / DMDHEU 80 / 35na bazi MgCl2 30Neionski14 BDMGU / DMDHEU 80 / 35na bazi Zn(NO3)230Neionski15CA 69SHP65//6BTCA 60SHP65// Tablica 5 - Utjecaj obrade protiv gu~vanja na stupanj bjeline i stupanj po~uenja celuloznih materijala Table 5 - Influence of DP finishing at WI and YI of cellulose material Apretura Bath CIE Stupanj bjeline (WI) CIE Whiteness index  Stupanj po~uenja (YI) Yelowness indexPamuk CottonViskoza ViscosePamuk CottonViskoza Viscose1 74,36145,43,50-13,112 A 75,34113,63,28-6,703 A 74,17110,63,96-5,284 A 74, 90155,13,83-15,25 71,3191,25,21-1,816 73,4298,54,88-2,17Neobraeni Untreated75,4557,43,1610,5 Tablica 6 - Utjecaj obrade protiv gu~vanja na fizikalna svojstva pamu nog materijala Table 6 - Influence of DP finishing at physical properties of cellulose material Apretura BathKut oporavka Wrinkle Recovery Angles (( 0+P)Zadr~ana prekidna vrstoa Tensile Strength retention (%)Otpornost na habanje (Br. ciklusa) Abrasion resistance (No. of cycles)1 19567115002 A 18666130003 A 17776165004 A 18070145005 17975160006 2057915000Neobraeni Untreated859011000 POPIS SLIKA Slika 1 - Formule primjenjenih umre~iva a Fig. 1 - Formulas of applied reactants: DMDHEU, etherified DMDHEU, DMGU, Citric acid (CA)  EMBED Excel.Chart.8 \s  Slika 2 - Oslobaanje formaldehida u vodi na pamu nom i viskoznom materijalu obraenim apreturom 4 (A=DMGU+ MgCl2 B= DMGU+ Zn(NO3)2). Fig. 2 - Formaldehyde release at cotton and viscose material treated with bath 4 (A=DMGU+ MgCl2 B= DMGU+ Zn(NO3)2).  Slika 3 - Promjena obojenja viskoznog materijala bojadisanog sa 0,2 % vinilsulfonskim reaktivnim bojilom (Bezaktiv V, Bezema), te obraenog sredstvima za obradu protiv gu~vanja (1=CA, 2=BTCA, 3=DMGU+MgCl2, 4=DMGU+Zn(NO3)2, 5=DMDHEU+ MgCl2, 6= DMDHEU+ Zn(NO3)2 , 7= DMGU/DMDHEU+ MgCl2 ). Fig. 3 - Shade changes of viscose material dyed with 0,2% VS reactive dye (Yellow, Red, Blue, Black, Bezaktiv V, Bezema) and treated with finishes 1-7 SUMMARY A Comparison of Conventional and New Ecologically Acceptable Durable Press Finishing Agents S. Bischof Vukuai, D. Katovi, I. Solja i Alternative chemistries have been explored to provide the same crosslinking performance using formaldehyde-free chemicals. The most recently introduced approach that requires more aggressive curing temperatures and a phosphorous containing catalyst is PCA crosslinking. These reactants form an anhydride between adjacent carboxyls, than anhydride reacts with the hydroxyl of the cellulose, producing an ester group crosslink that has a high stability and durability. Possibility of application DP finishing products with low formaldehyde content (modified DMDHEU) and formaldehyde free (FF) products (modified dimethyl glyoksalurea) has been investigated in this paper. Application of mixture of these products has lowered the content of free formaldehyde from ~ 1200 ppm, resulting from application of modified DMDHEU, to ~ 600 ppm (showed at fig. 2). Washing process after the treatment has further lowered the content of free formaldehyde to less than 20 ppm, which fulfils even the most rigid regulations on the allowed content of free formaldehyde on textile materials. The best results of WI have been obtained with N-methyl products and lower with applied PCA. Citric acid has shown the lowest results of WI, because of its greatest sensitivity to high curing temperatures. Under these temperatures it decomposes to unsaturated acids (aconite, itaconic and citraconic) whose double bonds are the main cause of the yellowness. Some of the PCA have shown equaly good, or even better, resilience effects compared to the conventional N-methylol agents. The greatest disadvantage of N-metylol products is tensile strength decrase, which have been partialy improved by application of etherified DMDHEU and significantly improved with the aplication of PCA. According to our investigations application of PCA has caused lowest shade changes after the DP treatment of dyed cellulose material. Greatest shade changes have been caused with the usage of Zn-nitrate catalyst (fig. 3 baths 4 and 6). Commercially, it is the modified DMDHEU (glicolated or methylated) that is still most used today. With these products the most popular catalysts are magnesium based ones. The negative aspect of the catalysts is that they induce degradation of the cellulose as indicated by the decrease in the tensile strength of cotton fabric. Conventional DP finishing agents which are still mostly applied products are tried to be maximally improved from the ecological point of view, since they are still in the usage primarily because of the economical reasons. Main alternatives to conventional N-methylated products are PCA, which are offering fulfilment of both ecologically and economically requirements. Some of these products have already been commercialised and represent the most recent technology to challenge the existing line of formaldehyde-based products. University of Zagreb, Faculty of Textile Technology, Department of Textile Chemistry and Material Testing Savska 16/5, 10 000 Zagreb, Croatia Popis kratica DP - Durable Press Finishing (obrada protiv gu~vanja) DMDHEU - dimetiloldihidroksietilen urea DMGU = DMeDHEU - dimetilglioksal urea PCA - polikarboksilna kiselina BTCA - 1,2,3,4-butantetrakarboksilna kiselina CA - citric acid (limunska kiselina) dE - ukupna promjena obojenja VS -vinilsulfonska WI - stupanj bjeline YI - stupanj po~uenja WRA - Wrinkle Recovery Angles (kut oporavka) Proaireni abstrakt U radu su istra~ivana alternativna sredstva za obradu protiv gu~vanja koja ne sadr~e formaldehid s ciljem postizanja jednako dobrih efekata umre~avanja. Sredstva koja se odnedavno uvode u praksu su polikarboksilne kiseline, a zahtijevaju viae temperature kondenzacije i katalizatore na bazi fosfora. Ti reaktanti formiraju anhidrid izmeu susjednih karboksilnih grupa, a u slijedeem stupnju anhidrid reagira sa celuloznim hidroksilom i daje estersko umre~enje visoke stabilnosti i postojanosti. Istra~ivala se mogunost primjene sredstava s niskom koli inom formaldehida (modificirana DMDHEU) i sredstava koja ne sadr~e formaldehid (DMGU). Primjenom kombinacije ovih sredstava postignuto je smanjenje slobodnog formaldehida sa 1200 ppm na 600 ppm (prikazano na sl. 2). Uvoenjem dodatnog postupka pranja smanjena je koli ina formaldehida i do 20 ppm, ato zadovoljava i najstro~e zahtjeve za dozvoljenu koli inu formaldehida na tekstilnim materijalima. Najbolji rezultati stupnja bjeline (WI) su postignuti primjenom sredstava na bazi N-metilolnih produkata, a neato loaiji primjenom polikarboksilnih kiselina. Limunska kiselina je dala najni~e rezultate stupnja bjeline zbog velike osjetljivosti na visoke termokondenzacijske temperature. Pod tim uvjetima limunska kiselina se raspada na nezasiene kiseline (akonitnu, itakonsku i citrakonsku) ije dvostruke veze su glavni uzrok po~uenja materijala. Neke od PCA su pokazale podjednako dobre ili ak i bolje efekte obrade, u usporedbi s klasi nim N-metilolnim sredstvima. Najvei nedostatak klasi nih sredstava je smanjenje prekidne sile ato je djelomi no poboljaano primjenom eterificirane DMDHEU, te zna ajno poboljaano primjenom PCA. Rezultati naaih istra~ivanja su pokazali da primjena PCA uzrokuje najmanje promjene obojenja na celuloznom materijalu obojadisanom reaktivnim bojilima. Najvee promjene obojenja dobivene su primjenom katalizatora na bazi Zn-nitrata (sl. 3 - apretura 4 i 6). U danaanje vrijeme se najviae primjenjuju sredstva na bazi DMDHEU (glikolirane ili metilirane) uz katalizatore na bazi Mg-klorida. Negativna strana ovih katalizatora je da uzrokuju degradaciju celuloze, ato su pokazali smanjeni rezultati prekidne vrstoe celuloznog materijala. Klasi na sredstva za obradu protiv gu~vanja koja su joa uvijek naj eae primjenjivana sredstva, nastoje se ato je mogue viae poboljaati s ekoloakog stanoviata, jer su u upotrebi prvenstveno iz ekonomskih razloga. Glavna alternativa klasi nim sredstvima na bazi N-metilola su PCA koje nude zadovoljenje ekoloakih i ekonomskih zahtjeva. Neki od tih produkata su ve komercijalizirani i predstavljaju veliki izazov dosadaanjoj tehnologiji zasnovanoj na primjeni sredstava koja sadr~e formaldehid. 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