DE1912180A1 - Process for making textile goods crease-resistant and dirt-repellent - Google Patents

Description

Badiseh © Aailia = - & Söüa-Fatoik AG

Our sign O ₀ Z ₀ 26 057 Rj / Be

6 700 Ludwigskafen, 10, Mars 1969

Procedure summed up to crease-proof and dirt-repellent macaeii

OLÄ I'extilgut

It is bling-innnt _; Sestilgut Iaiitterfest ausurustes. _; by impregnating it with agents which improve the crease resistance and which apply to the extilgi. c substances applied in Qagzrais ^ h of catalysts react IaSg ¹ To Das loana "as is well known, so g. see that the sextile giri impregnated with watery agents that enhance the emitter resistance, like the Eatalj / satorea (Ι ₅ gögebanenfalls' iiacb. Prolonged storage imd / oäsr Yerarbe ^ tiing su Eleiäungsstückan. Sidx · Sinleitimg the reaction to Semp-S / jators gvjisehen 120 vm < 200 ^ 0 ex ^ä - · bitst wirös öiaö as-dess Högli ebiceit ordered that in ^ des i & concise 2es ';; il _t | ut iiass, ck fco:;.:;. i? ollgeouollensöi Zanr ^ aMd odei? on a Reetfeucbtigicsit sv / ischen 4 imcl 15 ϊ ^ geti-oelmo'c' Lei aiässiger! Peraperatu ? ³ i-iid linger Versaiäi; ::. ^ Essential Ifeuclitiglceitsverluste sicli sslbst au übarl £. B _C : ^: i _v ΐ: 1β the 'reaction to the · desired extent «bgelci-jvan, l ^ -; \," .. r iiimo-isu cases you work au.el. · so that sau from ^^ '"ΐ'®'- ¹¹ ^ ® ^ -ΐ-Äem TIAD gegsbenenfall ^ ϋτιΐθΕ involvement - ~ iü2r Kuiselientroclrming Next the crease resistance irerfcesBeriia ^ ii means and then the Vernetaungskatalysatoren on the S'a; fergot £ ..: fbnngtc Ja n ^ whether. Type of the litter resistance Yerfceiä <si? N "n means m: A je naoii the selected working conditions r ^ act-sri with disssri known equipment experience the means predominantly with the fiber material under Yernetsung or predominantly with itself sslnst with the formation of high molecular bar-like substances = Sextile goods that have been lisitst after these bad events, have the power to ^! l @ l) rai? .ch. more strongly indicated: ^: i- / ösQ "ß. and to hold on to the dirt more strongly during washing than in the state of being equipped with equipment is still known, ß-, . means polymers on the fiber material AAFF ^ trisgöEp iaar dis RQiosfsstigkeit that Binreissfestiglcsit _s Vj'raSlälaElselt and ÖIS Soh © «© rf @ stigk © it ₉ which, for by ICnitt @ i 5i :: -.? ^ j :: 2iiEtir £ ig © a im sillgesoiaen botsäelitlioii suffer, too

^82/69 0 @ i © IG ^

BATH ORIGINAL

Tone ^ o

- 2 - QoSo 2β 057

sern.o For this Sv / eel · :: siud, for example, dispersions lyethylene. and everything from copolymers of ET = Me-amides? oii Ac ^ tX sänr-an end other, polymerizable s. Ver <= '.? E ^ \ ,: as inebsso ^ dsre acrylic acid esters !!, became known =, füileii ϋί.ν · 3 .lufKS y-ϊ very good, but has, in some. gei yi | C _^":;; ο se ■?"': -. ro: lt ivy -. '. en hehandel te ^ Seztilien su one ryyltleii. ! ^ AnsslimüL- irüg yäLr & nd the ir / asehene or treatmen-άΐ at s β s "-räsariif-'y liquids tend ... This verstärkrifv-, ^{oohsiütistarkeit;} is, t ßa; verh.i210.ern can successfully 'i-l'l.voüvc-ljmz:.?! · -? - ''". di3 aside from the monomers mentioned. nc el · .. öCielrs υοώ / Mo ^ om ^ rsa with at least two polymeri-ΐβύ 'Puppelbindiingiii s ^ tisaltenc DaheE ¹ they have at 1 ·!;' ■■■ 6-rfesta>? 3?: Ü3ti '^;"_>: 7 as .Mditiys to reduce the pa-

i ^ it -yli-a FA ⁷ Hi from ^ ^?:: - ·; provided DSII Teztilausriister more and more \ '.. _iLTiU.g;..! ; "·:;Ϊ́; ν1ϋίίη ku lisfern, which, although in üün? Fä:? G knit te? ¹ / ■ *" ■ '": _ ■?". ";^' R ^ rllst ^ t, which are , but soe ';: ry.lic :: - d-yr Troc-k .'- y, G - :. so :: iLutEurig v / ähr-end of use ■:;! · "'ί." ΐ £ ! .1-1.ΐΊϊο: - d y l ⁷ · :... s ^ yiscijnutzbarkeit in their behavior eiic ^ yiitts -; So boosted oil 'Cill ^ .L ^ iS i = _o äherii require-

Polymeric

Bssender? Sc! I ^ ia '; jig]: eito "i

s :: ¹ rJ.o! it "dr.i"t; l3 die über; eat. '"ί; 3: ΐβ Ey-.l; .iisuiif3"siltf;

sn textiles; the synthetic iss such auρ polyolefins, acrylic, sntöait ^ n or made up of them- SQhmu G3 so persistently that ^ "■ y / äsolisr?.;; ϊθΛΛ & 3: · ^; α mti; by ΌΙιθ- = ^L E ka.ilB ο

Ays tiös iife-Ji £ itGatsolj.r: T- - "ν" · li «^ ;. the? Poljea öyy .iBg'ä ^ ysiyjatsu So Ii y - :. χ Iai? "Sii :. Bsi a.iei"

249 a Yerfateen is known, yyn-ttoalteii ₅ so ausestl.st © B. _? that oh. leiofct'.wi; :: ici. gEt! nöIicli.e2? säab ^ a Yerfah2J © ii ~ ·; springs the seictiles yi ^ slrats.I, Tsat '; ^ «Y ;. inir ?. with Emu lsi =

t: .c5: y ^r Jiii: .j.3t -yjg

- 3

ORIGINAL.

- 3 - O.Z. ? 6 057

1812180

Laundry and dry cleaning all the faster; the higher the content of su / ui-eköi & poaeiite in the copolymer. The textiles are named according to the Jkngs / ben ?! Patent specification is good dirt-repellent if they have been finished with copolymers that sew at least 30. Polymerized $ acrylic acid containing "Hisea ^ olv'saijisate with 30 high acrylic acid contents give the 2eictilgut a iirv ~ r s wishes full and stiff hand"

It is now gefasaed., You class textile goods by impregnation with agents that improve the crease resistance, and with emulsion polymer i sat e: a from 13 to 60 fo at least one polymerisable en I-ϊοηο- or]): L carboxylic acid and 85 to 40 fo can make at least one further monomers and allowing the substances applied to the textile material to act in the manner of crosslinking catalysts very well crease-proof, seaiatitz-repellent and easily give off dirt _; without taking a troublesome Tarsteifung fabric hand in Eaiif rye 3iissöii ₅ 'nominal one than Smulsionspolymerisate used those which have been prepared in sswei polymerization stages so that in DER first polymerization 10 to 90 of the total weight fo all Koaomeren ₉ but no more than 40 fo the weight bxl caEboxylic acid-containing monomers and in the second stage the remaining proportions of the monomers were converted »

The emulsion copolymers to be used according to the invention are prepared by conventional emulsion polymerization processes. The emulsion of the copolymer produced in the first stage, which serves as a seed latex for the monomers of the second polymerisation stage, can be produced after the emulsion-based emulsion process and thus be a primary emulsion, but it can also be produced by emulsifying a suitable IsSsraigs-, Fällimgs- or Blockpolirmerisates are generated unö. then be a secondary emulsion. The polymerization of the remaining monomers in the second stage can be carried out continuously or discontinuously at any point in time, preferably immediately after the production of the seed latex.

The polymerization of the monomers from the

ÖD983S / §2 @ 4 - * -

BAD ORICnNAt.

- 4 - O = Zo 26 057

suitable emulsion polymers can be used in the presence of the usual Kili's fabrics and additives at 0 to 100 C using radical-forming starter systems can be carried out.

Polymerizable mono- and dicarboxylic acids include, for example, acrylic acid, Methacrylic acid, fumaric acid, maleic acid, crotonic acid, itacoic acid, and C-chloroacrylic acid. Acrylic acid, methacrylic acid and mixtures thereof are preferred.

Other monomers which are to be contained in the copolymer in an amount of 85 to 40% by weight are above all those which, when polymerized, form water-insoluble homopolymers; Of these, the "simple" monomers should be particularly emphasized, ie those which, apart from a double bond or conjugated double bond accessible for polymerization, contain no functional groups which cause crosslinking of the polymer during or after the polymerization. Such monomers are preferably the esters of acrylic and methacrylic acid, in particular those with low molecular weight alcohols, v / ie acrylic acid and many other methacrylic acid methyl, ethyl, n-propyl, i-propyl and butyl esters, for example the vinyl esters low molecular weight aliphatic carboxylic acids such as vinyl acetate, vinyl propionate and vinyl pivalate , vinyl halides such as vinyl chloride and vinylidene chloride, polymerizable hydrocarbons such as styrene and butadiene, acrylonitrile and methacrylonitrile.

Copolymers in which up to 5 / ί _5, preferably up to 2 fo, of the simple, water-insoluble homopolymers forming monomers have been replaced by the same percentage of one or more monomers with at least two polymerizable double bonds have proven particularly useful. Such monomers are, for example, Mebrf & cliester et , ß-unge saturate polymerizable carboxylic acids with polyhydric alcohols ₅ s "B _o those of Glykoien, such as butanediol diacrylate and Hexandioläimethacrylat, glycerol, v / ie glycerol di- and triacrylate, and pentaerythritol, vinyl and allyl esters <sC, ß-unsaturated polymerizable carboxylic acids, such as vinyl methacrylate and allyl acrylate ₉ Mehrfacbamides oC ₅ ß-unsaturated polymerizable carboxylic acids, if the methylene

00883-8 / 2204 ~ ^b "

bath

- 5 - CZ ₀ 26 057

bis-acrylamid and F ₅ II ⁹ .IP-Erisacrsrloyl-s ^ pernydrotriaisrn. » m \ l Mehrfachestei ³ polymerizable AlkGhole with melirbaeisoaeu carboxylic acids, such as diallyl phthalate,

Further copolymers which can be used according to the invention are obtained, 'v / em? aa.ii up to 10; ", preferably 2 big 6 ^ ner simple, water-insoluble homopolymers forming monomers by the same" percentage of one or more monomers crosslinkable when the copolymers are used !? © rseirst. These are monomers that except polymerizable double bonds reactive groups onthc "soldering, lie during eggs textile treatment together Rait other groups of the copolymers or Seztilguten Tsirbessernden agents and / or with the dia wrinkle resistance with the ^r üe: ctilmaterial react with crosslinking ^ Such monomers eirvl Z.3 H. -llkoxymetliylaiaide der Acryl = - ond methacrylic acid, acrylamium, methacrylamide, H-Äeryloylurea and in particular monomers, which contain sweet less than a polymerizable double bond an oßlorhydrinruppe, v / ie the Estar eier aoryl- ιπΛ Kötbilorpropand * 02? yl - (1 s 2), 2,3-2) ichlorobutanediol- (1,4), 3-chlorobutanediol- (1,2,4), 1 ₃ 4-dichlorobutanediol- (2,3) ₉ 3 ° 0hlor -2-MethTrlpropanediol- (1,2) and 3- = chloro--2-cb.lormetljyi-propaiidiol "(1,2) _o Instead of ready-made monomers of the letatgenanritan type in the production of the copolymers, they can also be polyrazitized Replace the corresponding amount of acrylic · = · or methacrylic acid and connect the resulting copolymer with an equivalent amount of Epieblorhy dr in ums et ζ en =>

In addition to the monomers mentioned can erfindungsgeiuäss au ■ used copolymers contain up to 20 $, preferably up to 10 tso one or more simple water-soluble homopolymers biläeiider Honomerer ₅ are dia free of Garbouüäuregruppen, aasteile the corresponding percentage of simple sv / asserwnlöslicbe Homopolymerisate.bildenden Monomers polymerized in eatbalteno MonoiaeEe of this kind are e.g. Yinyl- Bulion · jcmne nna S & lse der ¥ inylsulfonsäure ₉ Si-Yinylp3fri? OliclDn _J E ^ L ^ ZftojlpjszQllAonr, ^ -Hydroxjla.lgts © Bs 2 Eobleiistoffatomeii in the allsyl radical, such as S ₀ B, B ^ Jiz'atlvjlcoTjlam.'lß. oä® "£ f ^? = Ozyp3? opyl>; iQtlmes3flf: ®iö. ₉ further

BAD Of? K3INAC

- 6 - ü "Zo 26 057

-1 Q1 9 1 β Π

polymizable betaines, as Ie. DAS 1211156 "are described; _s or polymerizable salts such as F-Tinyl IP aiethylimida-Koliiim-methylsulf at or IT (ß-Trlisethylammoniuimätbyl) at acrylamidmetliylsulf.

DIs listed on I: ei lung <ϊ-3Γ vo ^ sTcboria. Monomers with min · = st3> i5 ^; s'vei polymerisable s: i ₇ olefinically unsaturated double bonds (Vsmetzer j, dir monomers with reactive groups that can enter into moli of the polymerization v'eme ^ surigsjeeaktioaen, and de :; water-dissolving, non-acidic monomers on the two olefinization giifen. i is. stopped be varied limits "it is XOgIiCb _5, the betrivfeiiaeii HOiaomeren Yollständig during dsr first or the second polymer stage u.m3usetzen ions. it is also possible, a ^ e monomers concerned only partially or aatsilmä-BBiG in eir- e: _ ^{: of} the - two polymerization stages umsusevseri = iii ^ 'Gacijeiaend ϊ · ϊ the success of the inventive term :' en is "i .'-: r _; dae. = * ^Γ - ^ clsn" olymsrislerbar ^ n gartonic acids in which it: ~ ^ -.- n St-j / e not "ii '^ r as ^ Q " p are polymerized,

I / xe QuQi .: explained Mis "Kpolvmerisate are applied together with soleben means, ^ .ie bsi sextilgnt, crs a ^ s cellulose best'fct or cellulose e; i \; iiält _; improve the crease resistance, Soleue Mi ti; si are in large:, 3ser Salil known not in use. It is "predominantly ι ·: ι where appropriate, decayed poly-F = methylolTerblndiTigen of Oarbamidsia, Thiocarbamöen and Amino-triasineu" for example "7on urea, Sliiobarnstoff, all mono urea, Sliiobarnstoff, ; , ii ^ Itfeylenlsarnstof 1 - Jf ₉ H ⁸ - !, 2 = Propylenh.a: - \ ästoff j E, Ή '-1,3-PrOpJ.l-snbt-rnsto-ff, 5 ~ Hyaro "yiieirabydrcpyrimi = don- 2, A-Hydroxy- and 4- ™ iiicox.y-5 ₅ 5-ciialkylhezali.yd5.Op3 / "riniiaonen with iii ed öi'niol ocular en alkyl and. Ailioxylgrnppen, Hexa.hyd2? O = 1 _s 3 _s 5 = triazincii = ° 2 "iiid its S-Alkyi- ^ s.ä S-Hydroisoxyalkyldrivaten with riiederiaclskulareri alkyl- oäey Hj-Srosyalkylgruppenj Glyoxaliaonourein, Uroiisii, Mono- and. ! DiurethBnsB, such as carbamic acid ethyl ester, Caruamiiisäure-propTl = ", -bntjl ^ imü-oetj-lester, Mca ^ bamin = acid-resistant tou l'ühylenglyJ: ol _s 1 ₅ 3"> ₂ 1, ^ Butsacliol and 1,6 = Hexaö = diol, Oarbaai:.: Isä; ire ~ ° - '> la Si. ^r "t - ili * '!'" e ^

BATH ORIGINAL

- 7 - U ₀ Zo 26 EAST

In addition to an optionally etherified IVVIethylolgruppe, substances which contain a reactive double bond or which contain several reactive double bonds or reactive groups of another kind, for example If-methylolacrylamide, N-methylolmethacrylamide, divinyl sulfone, methylenebisacsyiauiiä; F ₉ E ', M ^{! 5} -Iris ^ cryloyl "-3 ~ per! Iydrotriaziii _s Sris-ß-hydroxyätfeylsi-lfc" üiumsalse and eggs on the hydroxyl groups partly or completely with sulfuric acid ire rather te derivatives and Spiohlorhyarinc

The dre crease resistance improving agents are fo in the present process in conventional amounts of from 5 to 20, based on the 6-ewich.t of dry fiber material _s for this aufgebsaohtc

As crosslinking catalysts are in the usual way depending on Type of anti-crease agent either alkaline or latent alkaline catalysts or in most common acetalization catalysts, alkaline ones or latent alkaline catalysts are, for example, alkali hydroxides, Er dalkalih.y & r oxides and salts of weak inorganic compounds Or organic acids, such as carbonic acid, boric acid and acetic acid, with alkali metals, alkaline earth metals and strong organic acids Basenj as in Trialky! Amines.

Acetalization catalysts., Often somewhat imprecise as curing catalysts are acidic or latently acidic catalysts, For example, strong or medium-strength inorganic and organic acids, x- / ie hydrochloric acid, sulfuric acid, phosphoric acid, Oxalic acid, glycolic acid, maleic acid, monochloroacetic acid., Trichloroacetic acid, Tartaric acid and acetic acid, or salts which are not or only slightly acidic by nature, but by hydrolysis release acid or thermal influence, 2.B. Salts from ammonia, amines, or from hydroxides or oxides polyvalent Metals and medium-strength or, preferably, strong acids, such as ammonium chloride, ammonium sulfate, ammonium phosphate, ammonium nitrate , Dimonoethanolammonium hydrogen phosphate, ethanolammonium chloride s 1-hydroxy = 2 = -methyl = propylammonium-2-chloride, magnesium chloride, Aluminum chloride, zinc chloride, zinc nitrate, zirconium oxy-

BATH ORIGINAL

- 8 - U.Z. 26 057

Chloride and zinc fluorate. Depending on the chosen working conditions Individual crosslinking catalysts or mixtures of several crosslinking catalysts can be used in the customary manner. Known and The use of mixtures, for example, for crease-proof finishing when the material to be treated is partially dry, has proven its worth from acidic and latently acidic catalysts.

Me crosslinking catalysts are used in the present process in the usual amounts, ie generally in amounts of from 0.005 to 10 ^c / o, based on the weight of the dry fiber material.

The inventive method is carried out as it is from. Crease-proofing of textile material is known per se; from the

The only difference is that the fiber material to be finished is treated with the copolymers described in more detail above, in addition to the previously usual means. It has proven useful to use quantities from 0 _? 4 to 6 tfo of copolymers, calculated as powder substance and based on the weight of the dry fiber material, to be applied to this. For this purpose, the copolymers can be dissolved in organic solvents and the fiber material can be impregnated with these solutions; However, because of their simpler handling, aqueous baths containing the copolymers are preferred.

hold w. But it is also possible to use the copolymers from separate baths.

The finishing baths can also contain additives, for example oxyethylation products of higher alcohols, aqueous dispersions of polyethylene, silicic acid esters of higher alcohols, esters of aromatic polycarboxylic acids and higher alcohols and solutions Oxethylated polyamides, such as those commonly used for making textiles crease-proof, contain.

These additives can be used in the usual amounts, i.e. generally in a range of up to 10 ^σ />, based on the weight of the dry fiber = good.

009S33 / 22Ö4 ■. - 9 -

- 9 - C.E. 26 057

The fiber material impregnated with the finishing baths is depending on the the desired finishing result according to one of the aforementioned known working methods further treated, where appropriate the crosslinking catalysts retrospectively, from their own Baths are applied *

As fiber goods that are equipped according to the standard process, 7,, Ii, fibers, flocks, card sliver and particularly flat-shaped structures, such as unbound, non-bonded fiber fleeces, woven fabrics, knitted fabrics and braids, may be mentioned consist of pure natural or regenerated cellulose fibers, for example cotton, linen, rayon or rayon, or their mixtures with one another or with other fibers, for example with wool, silk, cellulose ester fibers or fibers made of synthetic polyamides, polyesters, polyolefins, acrylonitrile polymers or vinyl chloride polymers. The fiber material can also ^{consist of 100 c} / o fibers of synthetic high polymers or of mixtures of such synthetic fibers "

The method according to the invention is particularly suitable for finishing textile goods which consist of polyester fibers or which contain these in addition to other fibers, especially those made from natural or regenerated cellulose. Due to the hydrophobic character of the polyester fibers, such textile material tends to become very strong and stubborn soiling after use, which cannot be removed adequately by ITassv / äaebe. The dirt is removed smoothly if the textile material has been finished in accordance with the invention. The equipment is associated with an almost imperceptible change in grip? Fire protection; the result is a significantly lower stiffening of the erotiated textile material than when using emulsion mixtures for irrigation with the same gross composition, which are divided into conventional egg emulsion emulsion polymerisation. The pleasant, textile handle of the textile fabric equipped according to the invention generally makes a mechanical handle connection of the equipment superfluous

I) U; in the ßeiöpLolen, parts and percentages oind (Jewichtüeinheiten _o

ok

BATH ORIGINAL

- 10 - 0 _o 2, _o 26 057

_Ώ . . _{Ί Ί} 1912160

example 1

A white fabric 'ror ·. 115 g / m 2 of polyester / cotton (65 ₅ O 2 35.0) was impregnated with an aqueous liquor which

150 g / l of a 50 / I ^ en aqueous solution of IF ₉ I \ ['- Dimetbylol-

glyoxalsionou pure
125 g / l of an aqueous prepared as indicated below

Mixed polymer dispersion
40 g / l a- 40 csi-j ^ R. aqueous dispersion of tetra silica

sä.iisseste? ¹ <?. es Ta.Igfsttalkohols 25 ff / 1 MsCl, · 6 Ε, -Ό

2 g / l ÖMtianatrimPoP-lz of Ätbylendia.iniiiotetraacetic acid 20 g / l iuldulzt τοη 80 moles of ethylene oxide to 1 mole of sperm oil alcohol

contained, squeezed off bmx 65 ^c p FIottenau.fnähme, dried on the tenter at 100 "to HO ⁰ G to a residual moisture of 6 to 8 fo and condensed after one day of storage for 4 minutes at 150 ° C.

Dks so a.usgerüytets Sev / ev ^ seigts saasser a very good wash. and wear · Behavior a good balancing of impurities:

The (rsif / fifae was stained with coffee, tea, mustard, tomato ketchup, ink, lipstick and grease after normal washing in the drum washing machine at 60 ^J 0 gstr-ockuet and applied teaspoonful and applied ml on an area of about 5 cm in diameter is rubbed <3ri ₅ of the liquid substances, v / ^ de each 1 »Hach 24 stundiger Einwirküngsssit would berietst the fabric with water, the stained areas with a commercial liuushaltsv / ascbmittel coated and minute 15 after Einwirkungsaeit in a TromnielvraoebmaseMne in the conventional Prc = grams door normalvGraclinHi i; sfce laundry (-liquor) at 60 ⁰ O = washed, the fabric dried slid open (Mouoantobenotutigs Machino-dry 4-5) had ν.ηά no or only a few stains left, the irleekntellerr was according to the international fcab for äas Anbiuteri like fül- ^ c grade ti

Ι339 / 22ΘΙ »- Ii -

BATH

coffee 5 4th tomato 3 - tea 5 mustard 5 5 lipstick i - ink 5 Grease 4th

11 - O.Z. 26 057

That gives a total of 32.0 points out of a possible 35.

One that is equipped to match the same recipe, omitting the copolymer dispersion. Fabric achieved the same Monsanto rating for "wash and wear" behavior and a score of 27 for the removability of the stains _? 5 ·

The copolymer dispersion was prepared as follows:

According to the emulsion feed process at 85 C a mixture of 50 parts of ethyl acrylate, 0.25 parts of potassium persulfate, 0.4 parts of C-. [- Alkyl sulfonate and 90 parts of water in 60 minutes to a moving solution of I ₉ 25 parts of C-. - Added alkyl sulfonate and 0.25 part of potassium persulfate in 250 ropes of water. The polymerization is allowed to proceed at the same temperature up to 95 ° conversion, which takes about 15 minutes, calculated from the end of the feed, and a mixture of 125 parts of ethyl acrylate, 37.5 parts of acrylic acid, 37.5 parts of methacrylic acid, 2 parts of C is then added ^ _r -Alkylsulfonat, 0.25 parts of potassium persulfate and 370 parts of demineralized water in two hours at 85 ° C to the resulting polymer emulsion. It is allowed to polymerize for 60 minutes and a stable dispersion with 25 ° mixed polymer part is obtained. The k value (according to Fikentscher) of the copolymer is 95 »

Comparative experiment

A sample of the fabric mentioned in Example 1 was produced as indicated there using a mixed polymer dispersion from the same gross composition, the production of which is described below using the single-stage emulsion feed process,

& O983§ / 2204 - 12 -

- 12 - 0.2 ,. 26 057

equipped and tested. The finished product had an uncomfortable stiffness in contrast to the finished product according to Example 1 Handle. The test resulted in:

coffee 4th - 5th tomato 4th tea 5 mustard 4th - 5th lipstick 4th - • 5 ink VJl Grease 4th

The total number was 31.5 points.

The mixed polymer dispersion was prepared as follows

A solution of 1.25 parts of C 1-4 alkyl sulfonate, 0.25 parts of potassium persulfate and 250 parts of demineralized water is heated to 85 ° C uad in 3 hours at the same temperature and while stirring with the mixture of 175 parts of ethyl acrylate = esters, 37.5 parts each of acrylic acid and methacrylic acid, 2.4 parts of C-, I-alk: ylsulfonate, 0.50 parts of potassium persulfate and 460 parts fully demineralized water added. It is left to polymerize for an hour and a stable dispersion with a pesticide content is obtained 25 #. The k value (according to Mkent shear) of the copolymer is 89.

Example 2

A white fabric with 110 g / m made of polyester / cotton (67/33) was banded according to the recipe given in Example 1; a copolymer dispersion was also used, which is as follows was produced:

The mixture of 95 parts of ethyl acrylate, 5 parts of acrylic acid, 1 part of G ₁₅ -alkyl sulfonate, 0.25 part of potassium persulfate and 18C parts of deionized water became a solution of 1.25 parts of C - ^ - alkylsulfonate in 60 minutes at 85 ° C , 0.25 parts of potassium persulfate and 250 parts of demineralized water are added o

Ö09838 / 2204 _ _x ~.

BATH ORIGINAL

.- 13 - O.Z. 26 057

After 30 minutes the mixture of 80 parts of ethyl acrylate, 20 parts acrylic acid, 50 parts of methacrylic acid, 1.5 parts 0, ^ alkyl sulfonate, 0.25 part of potassium persulfate and 280 parts of water in two hours was added to the formed emulsion "at 87 ⁰ G was evenly added. After post-polymerization for one hour, a stable 25% polymer dispersion had formed. The k value (according to Fikentscher) of the polymer was 92.7.

The finished goods were characterized by being pleasantly soft Handle off.

The test of the soil release properties according to the example 1 resulted for:

dirt before B ev / ertu
after
1 η g
Machine wash (60 g)
χ 5 x 4 -
4 <
4th
4 -
4 - 3-in-l oil
!French dressing
Motor oil
Hot butter
Soy oil 5
4th
5
5
4th 5
-5 5
5
4 -
-5 4 - UlUI Example 3 mm mm
Il Il

A colorless fabric (110 g / m) made of cotton / polyester (50/50) was treated according to Example 1. The one used here The mixed polymer dispersion was prepared as follows:

Hot to a 85 ⁰ C solution of 1 part C - ,, - alkyl sulfonates 0.1 parts sodium vinyl sulfonate, 0.2 part of ammonium peroxydisulfate and 305 parts of deionized water was under vigorous stirring a mixture of 143.5 parts Itbylacrylat, 6.3 Parts of acrylic acid, 0.5 part of diallyl phthalate, 0.05 part of sodium vinyl sulfonate, 1.5 parts of C ₁ CC ₁₈ alkyl sulfonates, 15 parts of methacrylamide, 0.2 part of ammonium peroxydlsulfate and 220 parts of water are added. After 35 minutes, a second mixture of 51 parts of ethyl aorylate, 10 parts of methacrylamide, 35 parts of methaerylaic acid, 8 parts of acrylic acid, 0.25 parts of ammonium peroxydi-

009838/2204 -U-

BATH ORIGINAL

-U-

O.Z. 26 057

α hours

Sulphate and 230 parts of demineralized water were added in two at .85 ° C. to the polymer emulsion formed. The polymer emulsion formed after post-polymerization for one hour was 24.0 , the k value of the polymer was 113.5.

The test of the soil release properties was carried out as in example 1 stated carried out. The following results were obtained:

dirt

Grading before machine wash (60 C)

3-in-l oil
French dressing
Motor oil
Hot butter
Soy oil

4-5

4th-5th

The total number of points was 22.5, with a finish without the copolymer 17.0. The total score was after a machine wash at 60 G it is determined to be 22, which proves the excellent wash resistance of the soil release finish.

Similar good results were obtained with approximately 25 mixed polymer dispersions achieved, according to the instructions given in Example 3 from those given in Examples 4 to 8 Monomer combinations were made.

Example 4

Stage 1: 60 ^ of the total weight of all monomers; Mixture consisted from 81% by weight of ethyl acrylate, 9% by weight of acrylamide, 1 wt. ^ Diallyl phthalate, -9 wt.? S acrylic acid.

Level 2: $ 40 of the total weight of all monomers; mixture consisted of 50% by weight of ethyl acrylate, 5% by weight of styrene and 45% by weight methacrylic acid.

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Level 1: 50 tfo of the total weight of all monomers .; Mixture "consisted of 90% by weight of butyl acrylate, 5% by weight of vinyl carbazole, and 5% by weight of acrylic acid.

Level 2: $ 50 of the total weight of all monomers; Mixture consisted of 50 wt. Fo butyl acrylate, 5 wt. Fo vinylcarbazole, 10 wt. Fo acrylic acid and 35 wt. $ Methacrylic acid.

Example 6

Level 1: 40 fa of the total weight of all monomers; Mixture of 98 wt. $ Ethyl acrylate and 2 wt. $> Vinylpyrrolidone.

Stage 2: 60 % of the total weight of all monomers; Mixture of 50 wt. Io ethyl acrylate, vinyl acetate $ 5 wt., 2 wt. ^ Triallylformal, 0.5 wt. ^ Fatriumvinylsulfonat, 20 io itaconic acid and 22.5 wt. $ Methacrylic acid.

Example 7

Stage 1: 50 ^ of the total weight of all monomers; Mixture of 94 wt. Io butyl acrylate, 2 wt. $ F-methylolmethacrylamide and 4 6eWc $ acrylic acid.

Level 2; $ 50 of the total weight of all monomers; Mixture of 60 wt. $ Butyl acrylate, 2 wt. ^ U-methylolmethacrylamide, 5 wt. $ Butandiolmonoacrylat5 10 Gew.5 ^ acrylic acid and 23 wt. Io methacrylic acid.

Example 8

Step 1; 80 ia of the total weight of all monomers; Mixture of 95 wt. ^I / i ethyl acrylate, acrylic acid, and 4.5 $ 0.5 $ ITatriumacrylat wt...

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Level 2: $ 20 of the total weight of all monomers; Mix of 60 wt. ^ Methacrylic acid and 40 wt. ^ Acrylic acid.

Example 9

According to the equipment recipe given in Example 1, a

Cotton fabric (120 - 125 g / m) using a copolymer dispersion ", which was manufactured as specified there from the following components:

Stage 1: ZO fo of the total weight of all monomers; Mixture of 50% by weight each of butyl acrylate and methacrylic acid.

Stage 2: 80 % of the total weight of all monomers; Mixture of 62.5% by weight of butyl acrylate, 6.25% by weight of acrylic acid and 51.25% by weight of methacrylic acid.

Testing the soil release properties by means of the types of soil mentioned in Example 2 gave the finished fabric, the pleasantly soft feel of which was little changed by the finishing, the total number of points 24, which was still achieved after 5 machine washes at 60 ^° G.

Example 10

To. Finishing of a polyester fabric (110 g / m 2) according to Example 9, a total score of 22.5 was achieved in the soil release test. The handle of the finished fabric was very soft * By 5 Maseh.inenwasGh.en (60 ^G ö) the total score did not decrease.

Example 11

Bin polyester / Bäumwöllgewetie (50/50) with a square meter weight νάίι H5 g was made according to Example 1 using eggs Poiymerisätdispersioii ati & geifttstet, consisting of the following components manufactured according to the iiQ example 1 as given yer ferries been i

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Stage 1: 20 ψ> of the total weight of all monomers, feed of 100 wt / ^ ethyl acrylate as monomer.

Stage 2: $ 80 of the total weight of all monomers, monomer mixture from 62.5% by weight of ethyl acrylate and 37.5% by weight of equal amounts of acrylic and methacrylic acid.

The finishing result corresponded to that given in Example 1.

Example 12

A fine, white fabric (95 g / m) made of polyester / cotton (67/55) was finished and tested according to the recipe of Example 1 with modification of the copolymer dispersion. The polymer dispersion used for this example was prepared as follows:

At ^ 5 ⁰ C, the emulsion of 140 parts of ethyl acrylate, 2 parts of acrylic acid, 0.5 part of C-, ,, - alkyl sulfate, 0.1 part of Sodium acrylate, 0.1 part of potassium persulfate and 220 parts of distilled water in '10 minutes stirred in a solution of 2.5 parts of C, -, - alkyl sulfonate, 0.5 parts of sodium vinyl sulfonate, 0.3 parts of potassium persulfate and '' 0O parts of distilled water. Shortly thereafter, a second mixture of 5 parts of ethyl acrylate, 34 parts of methacrylic acid, 10 parts of acrylic acid, 1 part of C 1-4 alkyl sulfonate, 0.2 part of potassium perulfate. and 200 parts of distilled water, added to the polymer emulsion formed in 120 minutes. After about one hour of post-polymerization and steaming, a 26.3%, very stable polymer dispersion was obtained. kV / ert (according to Fikentscher) of the polymer: 90.

The test gave the excellent total number of points of 34 for the types of dirt mentioned in Example 1. After 5 machine washes, a total number of 32 points was determined. The total, -. pun-ktzahl was .'bei application of the listed in Example 2, Fettsor.ten 24, sewing machine washes five (60 ⁰ C) 23. The handle of the finished goods was much softer and therefore against-ro ,,, -. about , the untreated tissue changed much less

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than when using a copolymer dispersion of the same gross composition, but that according to the comparison test for example 1 was made in one step ..

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Claims (1)

- 19 - 0.7 ,. 26 057 Claim Process for making textile goods crease-resistant and dirt-repellent by impregnating with agents that improve crease resistance and with emulsion polymers 15 to 60 io of at least one polymerizable mono- or dicarboxylic acid and 85 to 40 $ of at least one further monomer and allowing the substances applied to the textile to react in the presence of crosslinking catalysts, characterized in that the emulsion polymers used are those which have been prepared in two polymerization stages so that in the first polymerization stage 10 to 90 % of the total weight of all monomers, but not more than 40 $ > the weight of the carboxylic acid group-containing monomers and in the second stage the remaining proportions of the monomers were converted. Badische Anilin- & Soda-Fabrik AG 009838/2204