EP0102930B1 - Wetting agent and its use as mercerising aid - Google Patents

Wetting agent and its use as mercerising aid Download PDF

Info

Publication number
EP0102930B1
EP0102930B1 EP83810399A EP83810399A EP0102930B1 EP 0102930 B1 EP0102930 B1 EP 0102930B1 EP 83810399 A EP83810399 A EP 83810399A EP 83810399 A EP83810399 A EP 83810399A EP 0102930 B1 EP0102930 B1 EP 0102930B1
Authority
EP
European Patent Office
Prior art keywords
component
wetting agent
agent according
carbon atoms
formula
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired
Application number
EP83810399A
Other languages
German (de)
French (fr)
Other versions
EP0102930A1 (en
EP0102930B2 (en
Inventor
Heinz Abel
Christian Guth
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Novartis AG
Original Assignee
Ciba Geigy AG
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Family has litigation
First worldwide family litigation filed litigation Critical https://patents.darts-ip.com/?family=4291874&utm_source=google_patent&utm_medium=platform_link&utm_campaign=public_patent_search&patent=EP0102930(B1) "Global patent litigation dataset” by Darts-ip is licensed under a Creative Commons Attribution 4.0 International License.
Application filed by Ciba Geigy AG filed Critical Ciba Geigy AG
Publication of EP0102930A1 publication Critical patent/EP0102930A1/en
Publication of EP0102930B1 publication Critical patent/EP0102930B1/en
Application granted granted Critical
Publication of EP0102930B2 publication Critical patent/EP0102930B2/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

Links

Classifications

    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/32Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/36Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/38Oxides or hydroxides of elements of Groups 1 or 11 of the Periodic Table
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10STECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S516/00Colloid systems and wetting agents; subcombinations thereof; processes of
    • Y10S516/01Wetting, emulsifying, dispersing, or stabilizing agents
    • Y10S516/03Organic sulfoxy compound containing

Definitions

  • the present invention relates to wetting agents which can be used in particular as mercerizing aids.
  • Mercerization is a common step in the processing of cellulosic fiber materials and concerns the treatment of these materials in aqueous alkaline liquors.
  • CH-A-192-832 describes e.g. Sulfuric acid esters of ethylene oxide adducts of aliphatic alcohols, which increase the wetting ability of the mercerizing liquors. According to CH-A-271-087, the wetting capacity of these fleets is increased by a mixture of alkyl sulfuric acids with certain alcohols and ethers. It is also known from DE-A-1-048-865 to use the sulfuric acid esters according to CH-A-192-832 in a mixture with a branched fatty alcohol as a wetting agent in the mercerization of cotton yarn.
  • the strongly alkaline mercerizing liquors containing these wetting agents have in many cases still insufficient net power.
  • these liquors can be used for gel formation, especially at lower temperatures and high alkali concentrations.
  • Your biggest disadvantage is in part very strong foam formation can be seen during the mercerization, which can impair working particularly on yarn mercerization machines.
  • the formation of voluminous foam layers also disturbs the concentration and recovery of the alkali lye from the wash baths following the mercerizing bath.
  • Wetting agents have now been found which, when used in mercerizing liquors, overcome the disadvantages mentioned and are notable for good wetting action and very little foaming.
  • the wetting agents according to the invention contain, in addition to a sulfuric acid ester of a fatty alcohol, e.g. of 2-ethyl-n-hexanol. and a phosphoric acid ester of a monoalcohol, e.g. of the butanol or isobutanol always a C6 - Cta alcohol, e.g. 2-ethyl-n-hexanol, and optionally a hydrotopant, e.g. 2,4-dihydroxy-2-methylpentane.
  • a sulfuric acid ester of a fatty alcohol e.g. of 2-ethyl-n-hexanol.
  • a phosphoric acid ester of a monoalcohol e.g. of the butanol or isobutanol always a C6 - Cta alcohol, e.g. 2-ethyl-n-hexanol, and optionally a hydrotopant, e.
  • the wetting agent known from BE-A-698 817 has an inadequate wetting effect, which manifests itself in a relatively low shrinking rate in the cotton.
  • the present invention furthermore relates to the use of the wetting agents in the mercerization of cellulose-containing fiber materials.
  • the phosphoric acid esters of a monoalcohol used as component (b) can be used as monoesters of the formula or as a mixture of the esters of the formulas (2a) and (2b).
  • the radicals R 2 contain 4 to 12, in particular 4 to 6, carbon atoms. Possible R 2 radicals are listed in the explanation for component (a). In addition, there are also residues of amyl and especially butyl alcohol.
  • the phosphoric acid esters can be used alone or as a (technical) mixture with one another. Monobutyl phosphate is particularly suitable.
  • component (c) can be used as component (c). These can also be used in the form of condensation products with paraformaldehyde [(CH 2 O) x ].
  • component (c) like components (a) and (b), can be used in the form of (technical) mixtures of the alcohols in question.
  • component (e)) is an adduct of an organopolysiloxane, preferably dimethylpolysiloxane and ethylene oxide or propylene oxide.
  • adducts can by the likely formula in which q is 3 to 50, preferably 3 to 25, r 2 or 3, s 0 to 15, t 1 to 25, x, 3 to 10 and R 3 .
  • Such polyether siloxanes are e.g. in DE ⁇ B ⁇ 1 719 238 and in US ⁇ A ⁇ 2 834 748, 3 389 160 and 3 505 377.
  • R 3 and R 4 are each alkyl having 1 to 4 carbon atoms, preferably methyl, a '1 to 20, b' 2 to 20, c '1 to 50, d' 1 or 2, preferably 1, and m 2 to 5 is.
  • siloxane compounds are described in DE-B-1 795 557.
  • siloxane compounds which have a cloud point of 20 to 70, in particular 25 to 50 ° C.
  • SILICONSURFACTANT L 546 0 (trademark) is suitable, for example, as a commercially available component (e) which corresponds to the probable formula (3) and has a cloud point of 32 ° C.
  • the wetting agents according to the invention can contain further components, e.g. Contain complexing agent (component (f)).
  • component (f) Contain complexing agent
  • Suitable components (f) preferably correspond to the formula wherein R, and R 2 independently of one another ⁇ CH 2 OH, ⁇ CHO or ⁇ CO 2 M, M is hydrogen or an alkali metal, preferably sodium, and x is 2 to 5.
  • Particularly preferred compounds of the formula (5) are hydroxycarboxylic acids of the formula wherein M and x have the meanings given, or a lactone of these hydroxycarboxylic acids. Gluconic acid and glucoheptanoic acid or their sodium salts show particularly good results.
  • Suitable hydrotroping agents preferably correspond to the formula wherein R 3 and R 4 are independently hydrogen or alkyl having 1 to 4 carbon atoms, especially methyl, and x 2 is 1 to 5.
  • x 2 1 and R 3 and R 4 are independently hydrogen or methyl.
  • a particularly valuable compound is 2-methyl-2,4-pentanediol.
  • wetting agents according to the invention which contain both component (f) and component (d) lead to particularly good results.
  • the combination of gluconic acid (sodium salt) / 2,4-dihydroxy-2-methylpentane should be mentioned in particular.
  • Components (a), (b), (c) and (d) and optionally (e) and / or (f) are preferably used in the form of an aqueous solution.
  • aqueous solutions of the wetting agents according to the invention preferably contain 5-50% of component (a), 0.5-30% of component (b), 0.5-5% of component (c), 5-15% of component ( d) and optionally 0.1-1% of component (e) and / or 0.1-5% of component (f).
  • component (a) Very suitable are those wetting agents that in aqueous solution 25-40% of component (a), 0.5-20% of component (b), 0.5-2% of component (c), 10-15% of the component (d) and optionally 0.1-0.5% of component (e) and / or 2-4% of component (f).
  • Particularly preferred wetting agents contain 30-35% of component (a), 0.5-10% of component (b), 1-1.5% of component (c), 10-15% of component (d) in aqueous solution. , 0.1-0.5% of component (e) and 2-4% of component (f).
  • the wetting agents according to the invention are suitable as auxiliaries in finishing processes of cellulose-containing fiber materials. In particular, they prove to be valuable wetting agents in the mercerization of these fiber materials.
  • 1-20 preferably 2.5-10 g of the above-mentioned aqueous solutions per liter of mercerizing liquor are used.
  • Cellulose fibers for example, have a higher gloss during mercerization. At the same time, their dye absorption capacity and tear resistance are improved.
  • the fibers are mixed with concentrated alkalis (approx. 22-28%), e.g. treated aqueous solutions of lithium, sodium or potassium hydroxide or mixtures of these hydroxides.
  • concentrated alkalis approximately 22-28%
  • the fibers can be subjected to simultaneous stretching, which further increases the gloss effect.
  • the temperature of the mercerizing liquors is preferably about 5 to 20 ° C.
  • the temperature of the mercerizing liquors is preferably about 5 to 20 ° C.
  • Cotton and blended fabrics with regenerated celluloses such as cellulose and rayon (rayon) are particularly suitable as cellulose-containing fiber materials.
  • regenerated celluloses such as cellulose and rayon (rayon) are particularly suitable as cellulose-containing fiber materials.
  • the mercerization of mixed fabrics made from native (e.g. cotton, as well as hemp and flax) and regenerated celluloses places high demands on the concentration and composition of the mercerizing liquors due to the divergent properties of these components. That is why blended fabrics almost become exclusively dry mercerized, which prevents additional (critical) contact of the mixed fabric with cooking or mesh baths.
  • the mercerization is carried out as yarn or piece mercerization.
  • a detailed description of these processes as well as the mercerization in general is e.g. in Lindner, Textile auxiliaries and washing raw materials,ticianliche Verlagsgesellschaft, Stuttgart, 1964, Volume 2, page 1474 ff.
  • wetting agents according to the invention in particular soche, which contain components (a) to (f), also allow quick and trouble-free recovery of the alkali from the (mercerizing) washing baths following the mercerizing bath.
  • soche which contain components (a) to (f)
  • these wetting agents have an extremely low tendency to foam.
  • the concentrated liquor obtained can then be reused in the mercerizing bath.
  • the wetting agents according to the invention are thus at least on a par with the prior art in terms of their wetting action, but also had the great advantage that they e.g. hardly have any tendency to foam in the case of the alkali recovery mentioned.
  • a cotton strand (weight: 1 g, length 24 cm), weighted with a weight of 33 g, is immersed in the filled cylinder and then the change in length of the strand is measured at equidistant time intervals.
  • the rate of shrinkage that can be determined from this is a measure of the effectiveness of the wetting agents used in the mercerizing liquor.
  • This example shows the foam behavior of the mercerizing liquors in the application using the glass cylinder shake test.
  • the wetting agent according to the invention completely suppresses foam formation.
  • the foam development in the lye recovery is significantly reduced by the wetting agent according to the invention compared to the comparison wetting agent.
  • This example shows the effectiveness of the wetting agents according to the invention in strongly alkaline mercerizing liquors.
  • Desized cotton fabric (square meter weight 180 g) is attached to a pin frame without tension and immersed for 1 minute in a mercerizing liquor containing 311.9 g sodium hydroxide solution per liter (which corresponds to a 25% solution) and 6 g of a wetting agent from (a) 80 % of a 40% aqueous solution of 2-ethylhexyl sulfate (sodium salt), (b) 3% of a 50% aqueous solution of monobutyl phosphate, (c) 1.3% 2-ethyl-n-hexanol, (e) 0.5 % Siloconsurfactant L 546 °, (f) 3.5% sodium gluconate and (d) 11.7% 2,4-dihydroxy-2-methyl-pentane.
  • the temperature of the mercerizing liquor is 18 ° C.
  • the mixture is then leached with hot water (70 ° C.) for 1 minute and treated with cold water which contains 5 ml / l acetic acid (40%).
  • the fabric is then rinsed, squeezed off on a padder and dried in a drying cabinet at 100 ° C. The gloss and the dyeability of the fabric are significantly improved.

Landscapes

  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical Or Physical Treatment Of Fibers (AREA)

Description

Die vorliegende Erfindung betrifft Netzmittel, die insbesondere als Mercerisierhilfsmittel verwendet werden können.The present invention relates to wetting agents which can be used in particular as mercerizing aids.

Die Mercerisation ist ein üblicher Schritt bei der Verarbeitung von cellulosehaltigen Fasermaterialien und betrifft die Behandlung dieser Materialien in wässrigen alkalischen Flotten.Mercerization is a common step in the processing of cellulosic fiber materials and concerns the treatment of these materials in aqueous alkaline liquors.

Für die Mercerisation geeignete Netzmittel sind schon seit langem bekannt. CH-A-192-832 beschreibt z.B. Schwefelsäureester von Aethylenoxidaddukten aliphatischer Alkohole, die die Netzfähigkeit der Mercerisierflotten erhöhen. Gemäss CH-A-271-087 wird das Netzvermögen dieser Flotten durch eine Mischung von Alkylschwefelsäuren mit gewissen Alkoholen und Aethern erhöht. Ferner ist aus DE-A-1-048-865 bekannt, die Schwefelsäureester gemäss CH-A-192-832 im Gemisch mit einem verzweigten Fettalkohol als Netzmittel bei der Mercerisation von Baumwollgarn einzusetzen.Wetting agents suitable for mercerization have been known for a long time. CH-A-192-832 describes e.g. Sulfuric acid esters of ethylene oxide adducts of aliphatic alcohols, which increase the wetting ability of the mercerizing liquors. According to CH-A-271-087, the wetting capacity of these fleets is increased by a mixture of alkyl sulfuric acids with certain alcohols and ethers. It is also known from DE-A-1-048-865 to use the sulfuric acid esters according to CH-A-192-832 in a mixture with a branched fatty alcohol as a wetting agent in the mercerization of cotton yarn.

Die diese Netzmittel enthaltenden stark alkalischen Mercerisierflotten besitzen jedoch ein in vielen Fällen noch unzureichendes Neztvermögen. Dazu kommt, dass insbesondere bei tieferen Temperaturen und hohen Laugenkonzentrationen diese Flotten zur Gelbildung niegen können. Ihr grösster Nachteil ist aber in der z.T. sehr starken Schaumbildung während der Mercerisation zu sehen, was das Arbeiten insbesondere auf Garnmercerisiermaschinen sehr beeinträchtigen kann. Ferner stört die Bildung voluminöser Schaumschichten auch die Aufkonzentrierung und Rückgewinnung der Alkalilauge aus den auf das Mercerisierbad folgenden Waschbädern.However, the strongly alkaline mercerizing liquors containing these wetting agents have in many cases still insufficient net power. In addition, these liquors can be used for gel formation, especially at lower temperatures and high alkali concentrations. Your biggest disadvantage is in part very strong foam formation can be seen during the mercerization, which can impair working particularly on yarn mercerization machines. Furthermore, the formation of voluminous foam layers also disturbs the concentration and recovery of the alkali lye from the wash baths following the mercerizing bath.

Unzureichende Netzwirkung und insbesondere zu starke Schaumbildung sind Nachteile, die sich vor allem in der Garnmercerisation und bei den modernen, schnell arbeitenden Mercerisiermaschinen auf drastische Weise bemerkbar machen. Da die zu mercerisierende Ware mit hoher Geschwindigkeit durch die Flotte bewegt wird, muss sie innerhalb einer kürzeren Zeit benetzt werden, als das bei langsamer arbeitenden Maschinen der Fall ist. Die höhere Durchlaufgeschwindigkeit des zu mercerisierenden Materials gibt in der Regel Anlass zu vermehrter Schaumbildung auf der Flotte. Bei der Garnmercerisation verhindert dies nicht nur die schnelle, sondern auch die gleichmässige Benetzung des Garns. Gleichzeitig steigt die Konzentration an Mercerisierlauge in den der Mercerisierflotte nachfolgenden Waschbädern schneller an. Dies bedeutet, dass bei kontinuierlicher Arbeitsweise pro Zeiteinheit eine grössere Menge an Lauge aus diesen Waschbädem zurückgewonnen werden muss. Die Durchführung sowohl der Mercerisation als auch der Laugenrückgewinnung innerhalb einer kürzeren Zeit ist aber nur dann möglich, wenn sich die Schaumbildung in Grenzen hält und das verwendete Netzmittel eine gute Netzwirkung besitzt.Inadequate wetting and, in particular, excessive foaming are disadvantages which are particularly noticeable in yarn mercerization and in modern, fast-working mercerizing machines. Since the goods to be mercerized are moved through the fleet at high speed, they must be wetted in a shorter time than is the case with slower machines. The higher throughput speed of the material to be mercerized usually gives rise to increased foaming on the liquor. In yarn mercerization, this not only prevents the yarn from wetting quickly, but also evenly. At the same time, the concentration of mercerizing liquor in the wash baths following the mercerizing liquor increases more rapidly. This means that with continuous operation, a larger amount of lye must be recovered from these wash baths per unit of time. However, it is only possible to carry out both the mercerization and the alkali recovery within a shorter time if the foam formation is limited and the wetting agent used has a good wetting effect.

Es wurden nun Netzmittel gefunden, die, in Mercerisierflotten eingesetzt, die genannten Nachteile überwinden und sich durch eine gute Netzwirkung und sehr geringe Schaumbildung auszeichnen.Wetting agents have now been found which, when used in mercerizing liquors, overcome the disadvantages mentioned and are notable for good wetting action and very little foaming.

Insbesondere offenbart BE―A―698 817 schaumarme Netzmittel zur Verwendung als Mercerisiermittel, die

  • - mindestens ein anionisches Tensid auf der Basis von Sulfaten oder Sulfonaten, vorzugsweise sulfonierte, aliphatische Kohlenwasserstoffe mit 6-18 Kohlenstoffatomen, z.B. Kokosfett-Dinatriumsulfonat, Schwefelsäure, ester eines technischen Octanolgemisches oder des 2-Aethyl-n-hexanols,
  • - mindestens einen sekundären Phosphorsäureester eines aliphatischen Alkohols in Salzform, z.b. Diisopropylphosphat-Natriumsalz oder Di(ß-äthoxyäthyl)-phosphat-Natriumsalz,
  • - gegebenenfalls einen tertiären Phosphorsäureester eines aliphatischen Alkohols, z.B. Triisobutylphosphat oder Tri(ß-äthoxyäthyl)-phosphat und
  • - gegebenenfalls einen primären Phosphorsäureester, z.B. Monoisobutylphosphat-Dinatriumsalz enthalten.
In particular, BE ― A ― 698 817 discloses low-foaming wetting agents for use as mercerizing agents
  • at least one anionic surfactant based on sulfates or sulfonates, preferably sulfonated, aliphatic hydrocarbons having 6-18 carbon atoms, for example coconut oil disodium sulfonate, sulfuric acid, ester of a technical octanol mixture or 2-ethyl-n-hexanol,
  • at least one secondary phosphoric acid ester of an aliphatic alcohol in salt form, eg diisopropyl phosphate sodium salt or di (β-ethoxyethyl) phosphate sodium salt,
  • - optionally a tertiary phosphoric acid ester of an aliphatic alcohol, for example triisobutyl phosphate or tri (ß-ethoxyethyl) phosphate and
  • - optionally contain a primary phosphoric acid ester, for example monoisobutyl phosphate disodium salt.

Im Gegensatz dazu enthalten die erfindungsgemässen Netzmittel neben einem Schwefelsäureester eines Fettalkohols, z.B. des 2-Aethyl-n-hexanols. und einem Phosphorsäureester eines Monoalkohols, z.B. des Butanols oder Isobutanols stets einen C6--Cta Alkohol, z.B. 2-Aethyl-n-hexanol, und gegebenenfalls ein Hydrotopierungsmittel, z.B. 2,4-Dihydroxy-2-methyl-pentan.In contrast, the wetting agents according to the invention contain, in addition to a sulfuric acid ester of a fatty alcohol, e.g. of 2-ethyl-n-hexanol. and a phosphoric acid ester of a monoalcohol, e.g. of the butanol or isobutanol always a C6 - Cta alcohol, e.g. 2-ethyl-n-hexanol, and optionally a hydrotopant, e.g. 2,4-dihydroxy-2-methylpentane.

Die aus BE-A-698 817 bekannten Netzmittelheisen eine unthreichende Netzwirkung auf, die sich in relativ niederin Schrumpfgeschwindigkeit un der Baumwolle äußert.The wetting agent known from BE-A-698 817 has an inadequate wetting effect, which manifests itself in a relatively low shrinking rate in the cotton.

Gegenstand der vorliegenden Erfindung sind daher Netzmittel, die

  • (a) Schwefelsäureester eines Fettalkohols mit 6 bis 18 Kohlenstoffatomen,
  • (b) Phosphorsäureester eines Monoalkohols mit 4 bis 12 Kohlenstoffatomen,
  • (c) Alkohole mit 6 bis 18. Kohlenstoffatomen oder deren Kondensationsprodukte mit Paraformaldehyd und gegebenenfalls
  • (d) ein Hydrotropierungsmittel
enthalten.The present invention therefore relates to wetting agents which
  • (a) sulfuric acid esters of a fatty alcohol with 6 to 18 carbon atoms,
  • (b) phosphoric acid esters of a monoalcohol with 4 to 12 carbon atoms,
  • (c) alcohols with 6 to 18 carbon atoms or their condensation products with paraformaldehyde and optionally
  • (d) a hydrotroping agent
contain.

Gegenstand der vorliegenden Erfindung ist ferner die Verwendung der Netzmittel bei der Mercerisation cellulosehaltiger Fasermaterialien.The present invention furthermore relates to the use of the wetting agents in the mercerization of cellulose-containing fiber materials.

Als Komponente (a) in den erfindungsgemässen Netzmitteln kommen Schwefelsäureester von Fettalkoholen der Formel

  • (1) R,-O-SO,H
in Betracht. Der Alkylrest R, in dieser Formel kann gesättigt oder ungesättigt, cyclisch, verzweigt- oder geradkettig sein. Er enthält 6 bis 18 Kohlenstoffatome und leitet sich z.B. von Hexanol, Heptanol sowie Octyl-, Nonyl- und Decylalkohol ferner auch vom Lauryl-, Myristyl-, Cetyl-, Stearyl- und Oleylalkohol ab. Bevorzugt sind die Schwefelsäureester von Fettalkoholen mit 6 bis 12, insbesondere 8 oder 9 Kohlenstoffatomen. Besonders gute Ergebnisse werden mit den Schwefelsäureestern von verzweigten Isomeren der genannten Alkohole erzielt, wie z.B. 2-Aethylhexanol, Trimethylhexanol und Trimethylnonylalkohol. Die genannten Schwefelsäureester können allein oder als (technisches) Gemisch untereinander in den erfindungsgemässen Netzmitteln eingesetzt werden.As component (a) in the wetting agents according to the invention there are sulfuric acid esters of fatty alcohols of the formula
  • (1) R, -O-SO, H
into consideration. The alkyl radical R in this formula can be saturated or unsaturated, cyclic, branched or be straight chain. It contains 6 to 18 carbon atoms and is derived, for example, from hexanol, heptanol and octyl, nonyl and decyl alcohol and also from lauryl, myristyl, cetyl, stearyl and oleyl alcohol. The sulfuric acid esters of fatty alcohols having 6 to 12, in particular 8 or 9, carbon atoms are preferred. Particularly good results are obtained with the sulfuric acid esters of branched isomers of the alcohols mentioned, such as 2-ethylhexanol, trimethylhexanol and trimethylnonyl alcohol. The sulfuric acid esters mentioned can be used alone or as a (technical) mixture with one another in the wetting agents according to the invention.

Die als Komponente (b) eingesetzten Phosphorsäureester eines Monoalkohols können als Monoester der Formel

Figure imgb0001
oder als Gemisch aus den Estern der Formeln (2a) und (2b) vorliegen.The phosphoric acid esters of a monoalcohol used as component (b) can be used as monoesters of the formula
Figure imgb0001
or as a mixture of the esters of the formulas (2a) and (2b).

Darin enthalten die Reste R2 4 bis 12, insbesondere 4 bis 6 Kohlenstoffatome. In Frage kommende Reste R2 sind in der Erläuterung für Komponente (a) aufgezählt. Hinzu kommen zusätzlich noch Reste von Amyl- und insbesondere Butylalkohol. Die Phosphorsäureester können allein oder auch als (technisches) Gemisch untereinander verwendet werden. Besonders geeignet ist Monobutylphosphat.The radicals R 2 contain 4 to 12, in particular 4 to 6, carbon atoms. Possible R 2 radicals are listed in the explanation for component (a). In addition, there are also residues of amyl and especially butyl alcohol. The phosphoric acid esters can be used alone or as a (technical) mixture with one another. Monobutyl phosphate is particularly suitable.

Als Komponente (c) können die unveresterten, in der Erläuterung für die Komponente (a) genannten Fettalkohole verwendet werden. Diese können auch in Form von Kondensationsprodukten mit Paraformaldehyd [(CH2O)x] verwendet werden. Die Komponente (c) kann wie die Komponenten (a) und (b) in Form von (technischen) Gemischen der in Frage kommenden Alkohole zur Anwendung kommen.The unesterified fatty alcohols mentioned in the explanation for component (a) can be used as component (c). These can also be used in the form of condensation products with paraformaldehyde [(CH 2 O) x ]. Component (c), like components (a) and (b), can be used in the form of (technical) mixtures of the alcohols in question.

Eine weitere Komponente, die in Kombination mit den genannten Komponenten (a) bis (d) verwendet werden kann (Komponente (e)), ist ein Addukkt aus einem Organopolysiloxan, vorzugsweise Dimethylpolysiloxan und Aethylen- oder Propylenoxid. Solche Addukte können durch die wahrscheinliche Formel

Figure imgb0002
dargestellt werden, worin q 3 bis 50, vorzugsweise 3 bis 25, r 2 oder 3, s 0 bis 15, t 1 bis 25, x, 3 bis 10 und R3. Alkyl mit 1 bis 4 Kohlenstoffatomen, vorzugsweise Methyl, istAnother component that can be used in combination with the components (a) to (d) mentioned (component (e)) is an adduct of an organopolysiloxane, preferably dimethylpolysiloxane and ethylene oxide or propylene oxide. Such adducts can by the likely formula
Figure imgb0002
in which q is 3 to 50, preferably 3 to 25, r 2 or 3, s 0 to 15, t 1 to 25, x, 3 to 10 and R 3 . Is alkyl of 1 to 4 carbon atoms, preferably methyl

Derartige Polyäthersiloxane sind z.B. in DE―B―1 719 238 sowie in US―A―2 834 748, 3 389 160 und 3 505 377 beschrieben.Such polyether siloxanes are e.g. in DE ― B ― 1 719 238 and in US ― A ― 2 834 748, 3 389 160 and 3 505 377.

Weitere Polyäthersiloxane, welche als fakultative Komponente (3) verwendet werden können, entsprechen der wahrscheinlichen Formel

Figure imgb0003
worin R3 und R4 je Alkyl mit 1 bis 4 Kohlenstoffatomen, vorzugsweise Methyl sind, a' 1 bis 20, b' 2 bis 20, c' 1 bis 50, d' 1 oder 2, vorzugsweise 1, und m 2 bis 5 ist.Other polyether siloxanes which can be used as optional component (3) correspond to the likely formula
Figure imgb0003
wherein R 3 and R 4 are each alkyl having 1 to 4 carbon atoms, preferably methyl, a '1 to 20, b' 2 to 20, c '1 to 50, d' 1 or 2, preferably 1, and m 2 to 5 is.

Derartige Siloxanverbindungen sind in DE-B-1 795 557 beschrieben.Such siloxane compounds are described in DE-B-1 795 557.

Bevorzugt sind nun solche Siloxanverbindungen, die einen Trübungspunkt von 20 bis 70, insbesondere von 25 bis 50°C aufweisen.Preference is now given to those siloxane compounds which have a cloud point of 20 to 70, in particular 25 to 50 ° C.

. Als handelsübliche Komponente (e), welche der wahrscheinlichen Formel (3) entspricht, und einen Trübungspunkt von 32°C aufweist, eignet sich z.B. SILICONSURFACTANT L 5460 (Handelsmarke).. SILICONSURFACTANT L 546 0 (trademark) is suitable, for example, as a commercially available component (e) which corresponds to the probable formula (3) and has a cloud point of 32 ° C.

Die erfindungsgemässen Netzmittel können weitere Komponenten, wie z.B. Komplexierungsmittel (Komponente (f)) enthalten.The wetting agents according to the invention can contain further components, e.g. Contain complexing agent (component (f)).

Geeignete Komponenten (f) entsprechen vorzugsweise der Formel

Figure imgb0004
worin R, and R2 unabhängig voneinander―CH2OH,―CHO oder―CO2M bedeuten, M Wasserstoff oder ein Alkalimetall, vorzugsweise Natrium, und x, 2 bis 5 ist.Suitable components (f) preferably correspond to the formula
Figure imgb0004
wherein R, and R 2 independently of one another ― CH 2 OH, ―CHO or ― CO 2 M, M is hydrogen or an alkali metal, preferably sodium, and x is 2 to 5.

Besonders bevorzugte Verbindungen der Formel (5) sind Hydroxycarbonsäuren der Formel

Figure imgb0005
worin M und x, die angegebenen Bedeutungen haben, oder ein Lacton dieser Hydroxycarbonsäuren. Gluconsäure und Glucoheptansäure bzw. ihre Natriumsalze zeigen besonders gute Resultate.Particularly preferred compounds of the formula (5) are hydroxycarboxylic acids of the formula
Figure imgb0005
wherein M and x have the meanings given, or a lactone of these hydroxycarboxylic acids. Gluconic acid and glucoheptanoic acid or their sodium salts show particularly good results.

Geeignete Hydrotropierungsmittel (Komponente (d)) entsprechen vorzugsweise der Formel

Figure imgb0006
worin R3 und R4 unabhängig voneinander Wasserstoff oder Alkyl mit 1 bis 4 Kohlenstoffatomen, insbesondere Methyl sind, und x2 1 bis 5 ist.Suitable hydrotroping agents (component (d)) preferably correspond to the formula
Figure imgb0006
wherein R 3 and R 4 are independently hydrogen or alkyl having 1 to 4 carbon atoms, especially methyl, and x 2 is 1 to 5.

In bevorzugten Verbindungen der Formel (7) ist x2 1 und R3 und R4 unabhängig voneinander Wasserstoff oder Methyl. Als besonders wertvolle Verbindung ist z.B. das 2-Methyl-2,4-pentandiol zu nennen.In preferred compounds of formula (7) x 2 1 and R 3 and R 4 are independently hydrogen or methyl. A particularly valuable compound is 2-methyl-2,4-pentanediol.

Erfindungsgemässe Netzmittel, die sowohl die Komponente (f) als auch die Komponente (d) enthalten, führen zu besonders guten Resultaten. Insbesondere ist in diesem Zusammenhang die Kombination Gluconsäure (Natriumsalz)/2,4-Dihydroxy-2-methyl-pentan zu erwähnen.Wetting agents according to the invention which contain both component (f) and component (d) lead to particularly good results. In this context, the combination of gluconic acid (sodium salt) / 2,4-dihydroxy-2-methylpentane should be mentioned in particular.

Die Komponenten (a), (b), (c) und (d) und gegebenenfalls (e) und/oder (f) werden vorzugsweise in Form einer wässrigen Lösung verwendet.Components (a), (b), (c) and (d) and optionally (e) and / or (f) are preferably used in the form of an aqueous solution.

$Vorzugsweise enthalten die wässrigen Lösungen der erfindungsgemässen Netzmittel 5-50% der Komponente (a), 0,5―30% der Komponente (b), 0,5-5% der Komponente (c), 5-15% der Komponente (d) und gegebenenfalls 0,1-1 % der Komponente (e) und/oder 0,1-5% der Komponente (f).The aqueous solutions of the wetting agents according to the invention preferably contain 5-50% of component (a), 0.5-30% of component (b), 0.5-5% of component (c), 5-15% of component ( d) and optionally 0.1-1% of component (e) and / or 0.1-5% of component (f).

Sehr geeignet sind solche Netzmittel, die in wässriger Lösung 25―40% der Komponente (a), 0,5―20% der Komponente (b), 0,5-2% der Komponente (c), 10-15% der Komponente (d) und gegebenenfalls 0,1-0,5% der Komponente (e) und/oder 2-4% der Komponente (f) enthalten.Very suitable are those wetting agents that in aqueous solution 25-40% of component (a), 0.5-20% of component (b), 0.5-2% of component (c), 10-15% of the component (d) and optionally 0.1-0.5% of component (e) and / or 2-4% of component (f).

Besonders bevorzugte Netzmittel enthalten in wässriger Lösung 30-35% der Komponente (a), 0,5-10% der Komponente (b), 1-1,5% der Komponente (c), 10-15% der Komponente (d), 0,1-0,5% der Komponente (e) und 2-4% der Komponente (f).Particularly preferred wetting agents contain 30-35% of component (a), 0.5-10% of component (b), 1-1.5% of component (c), 10-15% of component (d) in aqueous solution. , 0.1-0.5% of component (e) and 2-4% of component (f).

Die erfindungsgemässen Netzmittel eignen sich als Hilfsmittel bei Veredlungsprozessen cellulosehaltiger Fasermaterialien. Insbesondere erweisen sie sich als wertvolle Netzmittel bei der Mercerisation dieser Fasermaterialien. Zu diesem Zweck werden 1-20, vorzugsweise 2,5-10 g der oben genannten wässrigen Lösungen pro Liter Mercerisierflotte verwendet.The wetting agents according to the invention are suitable as auxiliaries in finishing processes of cellulose-containing fiber materials. In particular, they prove to be valuable wetting agents in the mercerization of these fiber materials. For this purpose 1-20, preferably 2.5-10 g of the above-mentioned aqueous solutions per liter of mercerizing liquor are used.

Cellulosefasern erhalten bei der Mercerisation beispielsweise einen höheren Glanz. Gleichzeitig werden ihre Farbstoffaufnahmefähigkeit sowie die Reissfestigkeit verbessert. Die Fasern werden dazu mit konzentrierten Laugen (etwa 22-28%), wie z.B. wässrigen Lösungen von Lithium-, Natrium- oder Kaliumhydroxid oder Mischungen dieser Hydroxide behandelt. Dabei können die Fasern einer gleichzeitigen Streckung unterworfen werden, wodurch sich eine weiter Steigerung des Glanzeffektes erreichen lässt.Cellulose fibers, for example, have a higher gloss during mercerization. At the same time, their dye absorption capacity and tear resistance are improved. For this purpose, the fibers are mixed with concentrated alkalis (approx. 22-28%), e.g. treated aqueous solutions of lithium, sodium or potassium hydroxide or mixtures of these hydroxides. The fibers can be subjected to simultaneous stretching, which further increases the gloss effect.

Vorzugsweise beträgt die Temperatur der Mercerisierflotten etwa 5 bis 20°C. Je nachdem, ob die Fasern in trockenem, vorgekochtem oder vorgenetztem Zustand mercerisiert werden, spricht man von der Trocken- oder Nassmercerisation. Besonders die Trockenmercerisation macht verständlicherweise die Verwendung von sehr wirksamen Netzmitteln erforderlich.The temperature of the mercerizing liquors is preferably about 5 to 20 ° C. Depending on whether the fibers are mercerized in the dry, pre-cooked or pre-wetted state, one speaks of the dry or wet mercerization. It is understandable that dry mercerization in particular requires the use of very effective wetting agents.

Als cellulosehaltige Fasermaterialien kommen vor allem Baumwolle und Mischgewebe mit Regeneratcellulosen wie z.B. Zellwollen und Kunstseiden (Reyon) in Frage. Die Mercerisation von Mischgeweben aus nativen (z.B. Baumwolle, sowie Hanf und Flachs) und regenerierten Cellulosen stellt aber auf Grund der auseinanderstrebenden Eigenschaften dieser Komponenten hohe Anforderungen an die Konzentration sowie Zusammensetzung der Mercerisierlaugen. Deshalb wird Mischgewebe fast ausschliesslich trocken mercerisiert, wodurch ein zusätzlicher (kritischer) Kontakt des Mischgewebes mit Koch- bzw. Netzbädern vermieden wird.Cotton and blended fabrics with regenerated celluloses such as cellulose and rayon (rayon) are particularly suitable as cellulose-containing fiber materials. However, the mercerization of mixed fabrics made from native (e.g. cotton, as well as hemp and flax) and regenerated celluloses places high demands on the concentration and composition of the mercerizing liquors due to the divergent properties of these components. That is why blended fabrics almost become exclusively dry mercerized, which prevents additional (critical) contact of the mixed fabric with cooking or mesh baths.

Technisch wird die Mercerisation als Garn- oder Stückmercerisation durchgeführt. Eine detaillierte Beschreibung dieser Verfahren sowie auch der Mercerisation im allgemeinen ist z.B. in Lindner, Textilhilfsmittel und Waschrohstoffe, Wissenschaftliche Verlagsgesellschaft, Stuttgart, 1964, Band 2, Seite 1474 ff gegeben.Technically, the mercerization is carried out as yarn or piece mercerization. A detailed description of these processes as well as the mercerization in general is e.g. in Lindner, Textile auxiliaries and washing raw materials, Wissenschaftliche Verlagsgesellschaft, Stuttgart, 1964, Volume 2, page 1474 ff.

Erfindungsgemässe Netzmittel, insbesondere soche, welche die Komponente (a) bis (f) enthalten, ermöglichen aber auch eine schnelle und störungsfreie Rückgewinnung der Lauge aus den auf das Mercerisierbad folgenden (Mercerisier-) Waschbädern. Beim Abdestillieren des Wassers aus diesen Bädern, wodurch eine Aufkonzentrierung der Lauge auf den Laugengehalt des Mercerisierbades erreicht wird, ziegen diese Netzmittel eine ausserordentlich geringe Tendenz zur Schaumbildung. Die erhaltene konzentrierte Lauge kann dann im Mercerisierbad wieder verwendet werden.However, wetting agents according to the invention, in particular soche, which contain components (a) to (f), also allow quick and trouble-free recovery of the alkali from the (mercerizing) washing baths following the mercerizing bath. When the water is distilled off from these baths, as a result of which the alkali is concentrated to the alkali content of the mercerizing bath, these wetting agents have an extremely low tendency to foam. The concentrated liquor obtained can then be reused in the mercerizing bath.

Die erfindungsgemässen Netzmittel zeigen sich also hinsichtlich ihrer Netzwirkung dem Stand der Technik mindestens ebenbürtig, wiesen aber darüber hinaus den grossen Vorteil auf, dass sie z.B. bei der erwähnten Laugenrückgewinnung kaum zur Schaumbildung neigen.The wetting agents according to the invention are thus at least on a par with the prior art in terms of their wetting action, but also had the great advantage that they e.g. hardly have any tendency to foam in the case of the alkali recovery mentioned.

Die folgenden Beispiele erläutern die Erfindung, ohne sie darauf zu beschränken. Teile und Prozente beziehen sich auf das Gewicht, sofern nicht anders angegeben.The following examples illustrate the invention without restricting it. Parts and percentages are by weight unless otherwise specified.

Beispiel 1example 1

In diesem Beispiel wird die Schrumpfgeschwindigkeit von Baumwolle in Mercerisierlaugen gemäss DIN 53987 (Entwurf Juli 1973) bestimmt. Danach wird ein Glaszylinder mit 150 ml einer auf 15°C abgekühlten Natronlauge (24%) gefüllt, die 5 g/1 des Netzmittels der nachfolgenden Zusammensetzung enthält:

  • (a) 23,75% Schwefelsäureester des 2-Aethyl-n-hexanols,
  • (b) 25,0% Phosphorsäureester des Butanols,
  • (c) 1,0% 2-Aethylhexanol und
  • (e) 0,25% Siliconsurfactant L 546* (Handelsmarke) sowie 50,0% Wasser.
In this example, the shrinking speed of cotton in mercerizing lye is determined according to DIN 53987 (draft July 1973). A glass cylinder is then filled with 150 ml of a sodium hydroxide solution (24%) cooled to 15 ° C., which contains 5 g / 1 of the wetting agent of the following composition:
  • (a) 23.75% sulfuric acid ester of 2-ethyl-n-hexanol,
  • (b) 25.0% phosphoric acid ester of butanol,
  • (c) 1.0% 2-ethylhexanol and
  • (e) 0.25% silicone surfactant L 546 * (trademark) and 50.0% water.

Ein Baumwollstrang (Gewicht: 1 g, Länge 24 cm), der mit einem Gewicht von 33 g beschwert ist, wird in den gefüllten Zylinder eingetaucht und dann die Längenänderung des Stranges in äquidistanten Zeitintervallen gemessen. Die daraus ermittelbare Schrumpfgeschwindigkeit ist ein Mass für die Wirksamkeit der in der Mercerisierlauge verwendeten Netzmittel.A cotton strand (weight: 1 g, length 24 cm), weighted with a weight of 33 g, is immersed in the filled cylinder and then the change in length of the strand is measured at equidistant time intervals. The rate of shrinkage that can be determined from this is a measure of the effectiveness of the wetting agents used in the mercerizing liquor.

Zum Vergleich wird eine Mercerisierlauge verwendet, die als Netzmittel nur 5 g/l des Schwefelsäureesters des 2-Aethyl-n-hexanols enthält, und die Schrumpfgeschwindigkeit eines gleichen Baumwollstrangs bestimmt. Die Ergebnisse sind in den Tabellen 1a) und 1b) zusammengefasst.

Figure imgb0007
Figure imgb0008
For comparison, a mercerizing liquor is used which contains only 5 g / l of the sulfuric acid ester of 2-ethyl - n-hexanol as the wetting agent and which determines the rate of shrinkage of an identical cotton strand. The results are summarized in Tables 1a) and 1b).
Figure imgb0007
Figure imgb0008

Durch Verwendung von z.B. 5 g/1 des erfindungsgemässen Netzmittels erhält man nach bereits 30 Sekunden eine höhere Schrumpfung als mit dem Vergleichsnetzmittel nach 50 Sekunden.By using e.g. 5 g / l of the wetting agent according to the invention gives a higher shrinkage after only 30 seconds than with the comparison wetting agent after 50 seconds.

Beispiel 2Example 2

Dieses Beispiel zeigt das Schaumverhalten der Mercerisierflotten in der Applikation anhand des Glaszylinderschütteltests.This example shows the foam behavior of the mercerizing liquors in the application using the glass cylinder shake test.

100 ml Natronlauge (24%), die 1 bzw. 2 g/l des in Beispiel 1 verwendeten Netzmittels enthält, werden in einen Glaszylinder eingefüllt und auf einen Temperatur von 25°C gebracht. Der Glaszylinder wird dann 1 Minute kräftig geschüttelt und die Höhe des entstandenen Schaums nach bestimmten Zeiten gemessen.100 ml of sodium hydroxide solution (24%), which contains 1 or 2 g / l of the wetting agent used in Example 1, are introduced into a glass cylinder and brought to a temperature of 25 ° C. The glass cylinder is then shaken vigorously for 1 minute and the height of the foam formed is measured after certain times.

Zum Vergleich wird auch das Schaumverhalten einer Mercerisierflotte untersucht, die anstelle des oben verwendeten Netzmittels 1 bzw. 2 g/l des Schwefelsäureesters des 2-Aethyl-n-hexanols enthält. Die Ergebnisse sind aus der Tabelle 2 ersichtlich.

Figure imgb0009
For comparison, the foam behavior of a mercerizing liquor is also investigated, which contains 1 or 2 g / l of the sulfuric acid ester of 2-ethyl-n-hexanol instead of the wetting agent used above. The results are shown in Table 2.
Figure imgb0009

Während das Vergleichsnetzmittel z.T. sehr grosse Schaumhöhen zulässt, unterdrückt das erfindungsgemässe Netzmittel die Schaumbildung vollständig.While the comparison wetting agent partly allows very large foam heights, the wetting agent according to the invention completely suppresses foam formation.

Beispiel 3Example 3

Dieses Beispiel zeigt das Schaumverhalten eines nach der Mercerisierung verwendeten Waschbades bei der Laugenrückgewinnung.

  • Aus 500 ml verdünnter Mercerisierlauge (15%), die
  • 300 ml Natronlauge (24%)
  • 5 g/I Netzmittel gemäss Beispiel 1 und
  • 192,5 ml Wasser
enthält, wird am Rotationsverdampfer bei etwa 10-20 mbar solange Wasser abdestilliert, bis die Laugenkonzentration wieder 24% beträgt. Während der Destillation wird die Höhe des entstandenen Schaums in Abhängigkeit von der Zeit gemessen.This example shows the foaming behavior of a washing bath used after the mercerization in the recovery of lye.
  • From 500 ml of diluted mercerizing solution (15%), the
  • 300 ml sodium hydroxide solution (24%)
  • 5 g / l of wetting agent according to Example 1 and
  • 192.5 ml of water
contains, water is distilled off on a rotary evaporator at about 10-20 mbar until the alkali concentration is again 24%. During the distillation, the amount of foam produced is measured as a function of time.

Zum Vergleich wird dieser Vorgang mit 500 ml Mercerisierlauge, die 5 g/I des Schwefelsäureesters des 2-Aethyl-n-hexanols als Netzmittel enthält, wiederholt.

Figure imgb0010
For comparison, this process is repeated with 500 ml of mercerizing solution, which contains 5 g / l of the sulfuric acid ester of 2-ethyl-n-hexanol as a wetting agent.
Figure imgb0010

Die Schaumentwicklung bei der Laugenrückgewinnung wird durch das erfindungsgemässe Netzmittel gemessen am Vergleichsnetzmittel deutlich herabgesetzt.The foam development in the lye recovery is significantly reduced by the wetting agent according to the invention compared to the comparison wetting agent.

Beispiel 4Example 4

Dieses Beispiel zeigt die Wirksamkeit der erfindungsgemässen Netzmittel in stark alkalischen Mercerisierflotten.This example shows the effectiveness of the wetting agents according to the invention in strongly alkaline mercerizing liquors.

Entschlichtetes Baumwollgewebe (Quadratmetergewicht 180 g) wird ohne Spannung auf einem Nadelrahmen befestigt und während 1 Minute in eine Mercerisierflotte getaucht, die pro Liter 311,9 g Natronlauge (was einer 25%igen Lösung entspricht) und 6 g eines Netzmittels aus (a) 80% einer 40%igen wässrigen Lösung von 2-Aethylhexylsulfat (Natriumsalz), (b) 3% einer 50%igen wässrigen Lösung von Monobutylphosphat, (c) 1,3% 2-Aethyl-n-hexanol, (e) 0,5% Siloconsurfactant L 546°, (f) 3,5% Natriumgluconat und (d) 11,7% 2,4-Dihydroxy-2-methyl-pentan enthält. Die Temperatur der Mercerisierflotte beträgt 18°C.Desized cotton fabric (square meter weight 180 g) is attached to a pin frame without tension and immersed for 1 minute in a mercerizing liquor containing 311.9 g sodium hydroxide solution per liter (which corresponds to a 25% solution) and 6 g of a wetting agent from (a) 80 % of a 40% aqueous solution of 2-ethylhexyl sulfate (sodium salt), (b) 3% of a 50% aqueous solution of monobutyl phosphate, (c) 1.3% 2-ethyl-n-hexanol, (e) 0.5 % Siloconsurfactant L 546 °, (f) 3.5% sodium gluconate and (d) 11.7% 2,4-dihydroxy-2-methyl-pentane. The temperature of the mercerizing liquor is 18 ° C.

Anschliessend wird 1 Minute mit heissem Wasser (70°C) entlaugt und mit kaltem Wasser, das 5 ml/l Essigsäure (40%) enthält, behandelt. Das Gewebe wird dann nachgespült, auf einem Foulard abgequetscht und im Trockenschrank bei 100°C getrocknet. Der Glanz und die Anfärbbarkeit des Gewebes sind deutlich verbessert.The mixture is then leached with hot water (70 ° C.) for 1 minute and treated with cold water which contains 5 ml / l acetic acid (40%). The fabric is then rinsed, squeezed off on a padder and dried in a drying cabinet at 100 ° C. The gloss and the dyeability of the fabric are significantly improved.

Claims (14)

1. A wetting agent which contains
(a) sulfates of a fatty alcohol having 6 to 18 carbon atoms,
(b) phosphates of a monoalcohol having 4 to 12 carbon atoms,
(c) alcohols having 6 to 18 carbon atoms or condensation products thereof with paraformaldehyde and, optionally,
(d) a hydrotrope.
2. A wetting agent according to claim 1, which additionally contains - as component (e) - an adduct of an organopolysiloxane and ethylene oxide and/or propylene oxide and/or - as component (f) - a complexing agent.
3. A wetting agent according to claim 1, which contains - as component (a) - sulfates of a fatty alcohol having 6 to 12 carbon atoms.
4. A wetting agent according to claim 1, which contains - as component (b) - phosphates of a monoalcohol having 4 to 6 carbon atoms.
5. A wetting agent according to claim 1, which contains - as component (c) - an alcohol having 6 to 12 carbon atoms.
6. A wetting agent according to claim 1, which contains - as component (d) - a compound of the formula
Figure imgb0019
in which each of R3 and R4 independently of the other is hydrogen or alkyl having 1 to 4 carbon atoms, and x2 is 1 to 5.
7. A wetting agent according to claim 6, which contains - as component (d) - a compound of the formula
Figure imgb0020
in which each of R3 and R4 independently of the other is hydrogen or methyl.
8. A wetting agent according to claim 7, which contains - as component (d) - 2-methyl-2,4-pentanediol.
9. A wetting agent according to claim 2, which contains - as component (e) - an adduct of a dimethylpolysiloxane and ethylene oxide and/or propylene oxide.
10. A wetting agent according to claim 2, which contains - as component (f) - a compound of the formula
Figure imgb0021
in which each of R, and R2 independently of the other is ―CH2OH, -CHO or ―CO2M, M is hydrogen or an alkali metal, and x, is 2 to 5.
11. A wetting agent according to claim 10, which contains - as component (f) - a compound of the formula
Figure imgb0022
in which M and x, are as defined in claim 10.
12. A wetting agent according to claim 11, which contains - as component (e) - the sodium salt of gluconic acid.
13. A wetting agent according to any one of claims 1 to 12, which is in the form of an aqueous solution of components (a) to (d) and, optionally, (e) and/or (f).
14. A process for mercerising cellulosic fibre materials, which comprises using a wetting agent according to any one of claims 1 to 13.
EP83810399A 1982-09-08 1983-09-02 Wetting agent and its use as mercerising aid Expired - Lifetime EP0102930B2 (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
CH533682 1982-09-08
CH5336/82 1982-09-08

Publications (3)

Publication Number Publication Date
EP0102930A1 EP0102930A1 (en) 1984-03-14
EP0102930B1 true EP0102930B1 (en) 1986-10-15
EP0102930B2 EP0102930B2 (en) 1990-09-19

Family

ID=4291874

Family Applications (1)

Application Number Title Priority Date Filing Date
EP83810399A Expired - Lifetime EP0102930B2 (en) 1982-09-08 1983-09-02 Wetting agent and its use as mercerising aid

Country Status (6)

Country Link
US (1) US4494952A (en)
EP (1) EP0102930B2 (en)
BR (1) BR8304842A (en)
CA (1) CA1217006A (en)
DE (1) DE3366978D1 (en)
ZA (1) ZA836657B (en)

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4844710A (en) * 1986-12-08 1989-07-04 Ciba-Geigy Corporation Aqueous textile assistant of high storage stability and hard water resistance
EP0638685B1 (en) * 1993-08-10 1998-12-23 Ciba SC Holding AG Welling agent for mercerising
ES2182880T3 (en) * 1994-08-11 2003-03-16 Ciba Sc Holding Ag COMPOSITIONS OF MULTIFUNCTIONAL TEXTILE AGENTS.

Family Cites Families (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CH192832A (en) * 1936-03-24 1937-09-15 Chem Fab Vormals Sandoz Process for increasing the wetting and penetrating effect of alkalizing liquids by at least 15 o Bé.
CH271087A (en) 1948-12-15 1950-10-15 Ciba Geigy Process for increasing the wetting ability of mercerising liquors.
BE495124A (en) * 1949-04-13
BE536296A (en) 1954-03-22
CH345323A (en) * 1956-04-11 1960-03-31 Ciba Geigy Preparation for increasing the wetting power of mercerising liquors
DE1795557C3 (en) 1961-05-27 1974-10-03 Th. Goldschmidt Ag, 4300 Essen Process for the preparation of polyalkyl silicic acid esters with a polymer distribution which approximates the statistical equilibrium. Eliminated from: 1445364
BE666745A (en) 1964-07-14 1966-01-12
GB1143206A (en) 1965-02-08 1969-02-19 Union Carbide Corp Siloxane-oxyalkylene co-polymers
US3449261A (en) * 1966-02-01 1969-06-10 Fmc Corp Non-foaming wetting agents
US3505377A (en) 1966-08-12 1970-04-07 Union Carbide Corp Siloxane-oxyalkylene copolymer foam stabilizers
DE1619040B2 (en) * 1967-02-02 1974-01-24 Farbwerke Hoechst Ag, Vormals Meister Lucius & Bruening, 6000 Frankfurt Wetting agent for alkaline baths
BE698817A (en) * 1967-05-22 1967-11-03
DE2231148A1 (en) * 1972-06-26 1974-01-31 Hoechst Ag LAUGATING AND MERCERIZING SOLUTIONS

Also Published As

Publication number Publication date
BR8304842A (en) 1984-04-24
DE3366978D1 (en) 1986-11-20
CA1217006A (en) 1987-01-27
EP0102930A1 (en) 1984-03-14
EP0102930B2 (en) 1990-09-19
ZA836657B (en) 1984-04-25
US4494952A (en) 1985-01-22

Similar Documents

Publication Publication Date Title
DE69835769T2 (en) HIGH ALKALINE COMPOSITIONS CONTAINING HEXYL GLYCOSIDE AS HYDROTROP
DE2943754A1 (en) FOAM ABSORBERS AND THEIR USE FOR DEFOAMING AQUEOUS SYSTEMS
EP0420802B1 (en) Aqueous, storage stable, low foaming wetting agent
DE2418351A1 (en) PROCESS AND COMPOSITION FOR TEXTILE BLEACHING
EP0170144B1 (en) Washing process for sensitive textiles
EP1149945A1 (en) Composition for the pretreatment of fibrous materials
EP0360736B1 (en) Aqueous wetting and detergent composition stable in hard water, its production and use in textile pretreatment
EP0513571A1 (en) Improvements for the application by spraying of aqueous treating liquids on textile materials
EP0102930B1 (en) Wetting agent and its use as mercerising aid
EP0274350B1 (en) Aqueous storage-stable auxiliary textile agent resistant to hard water
EP0094656A2 (en) Process for simultaneously desizing and bleaching textile materials made of cellulosic fibres
EP0638685B1 (en) Welling agent for mercerising
EP0589978B1 (en) Use of special alkyl glycosides as auxiliaries in the pretreatment of textiles
DE3823454A1 (en) MERCERIZING AND / OR LYING AGENT
DE1245898C2 (en) Low-foaming, leveling wetting agent
EP0112801A1 (en) Magnesium complexes of oligomeric phosphonic-acid esters, process for their preparation and their use as stabilizers in bleaching baths containing alcaline peroxide
DE2903134B2 (en) Process for washing dyed or printed textiles
DE1617136B1 (en) Process for dry cleaning of textiles
EP0460036B1 (en) Single-bath degumming and decolorizing of natural silks
DE2326364A1 (en) SOLVENT BLEACHING PROCESS
DE2113211C3 (en) Mixture of surfactants
EP0205088A2 (en) Washing process for delicate textiles
DE3230101A1 (en) Alkali-dry process for natural cellulose fibres and their blends with synthetic fibres
DE2157061C3 (en) Process for pre-cleaning and bleaching textile materials
EP0716180A1 (en) Wetting agent for mercerizing

Legal Events

Date Code Title Description
PUAI Public reference made under article 153(3) epc to a published international application that has entered the european phase

Free format text: ORIGINAL CODE: 0009012

17P Request for examination filed

Effective date: 19830905

AK Designated contracting states

Designated state(s): BE CH DE FR GB IT LI

GRAA (expected) grant

Free format text: ORIGINAL CODE: 0009210

AK Designated contracting states

Kind code of ref document: B1

Designated state(s): BE CH DE FR GB IT LI

REF Corresponds to:

Ref document number: 3366978

Country of ref document: DE

Date of ref document: 19861120

ITF It: translation for a ep patent filed
ET Fr: translation filed
PLBI Opposition filed

Free format text: ORIGINAL CODE: 0009260

26 Opposition filed

Opponent name: HUELS AKTIENGESELLSCHAFT

Effective date: 19870703

PUAH Patent maintained in amended form

Free format text: ORIGINAL CODE: 0009272

STAA Information on the status of an ep patent application or granted ep patent

Free format text: STATUS: PATENT MAINTAINED AS AMENDED

27A Patent maintained in amended form

Effective date: 19900919

AK Designated contracting states

Kind code of ref document: B2

Designated state(s): BE CH DE FR GB IT LI

ITF It: translation for a ep patent filed
EN3 Fr: translation not filed ** decision concerning opposition
ET3 Fr: translation filed ** decision concerning opposition
REG Reference to a national code

Ref country code: FR

Ref legal event code: BR

ITTA It: last paid annual fee
REG Reference to a national code

Ref country code: CH

Ref legal event code: PUE

Owner name: CIBA-GEIGY AG TRANSFER- CIBA SC HOLDING AG

BECN Be: change of holder's name

Effective date: 19961129

REG Reference to a national code

Ref country code: FR

Ref legal event code: TP

REG Reference to a national code

Ref country code: GB

Ref legal event code: 732E

REG Reference to a national code

Ref country code: CH

Ref legal event code: PFA

Free format text: CIBA SC HOLDING AG TRANSFER- CIBA SPECIALTY CHEMICALS HOLDING INC.

REG Reference to a national code

Ref country code: FR

Ref legal event code: CD

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: FR

Payment date: 20010727

Year of fee payment: 19

Ref country code: CH

Payment date: 20010727

Year of fee payment: 19

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: DE

Payment date: 20010810

Year of fee payment: 19

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: GB

Payment date: 20010823

Year of fee payment: 19

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: BE

Payment date: 20011119

Year of fee payment: 19

REG Reference to a national code

Ref country code: GB

Ref legal event code: IF02

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: GB

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20020902

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: LI

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20020930

Ref country code: CH

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20020930

Ref country code: BE

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20020930

BERE Be: lapsed

Owner name: *CIBA SPECIALTY CHEMICALS HOLDING INC.

Effective date: 20020930

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: DE

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20030401

GBPC Gb: european patent ceased through non-payment of renewal fee

Effective date: 20020902

REG Reference to a national code

Ref country code: CH

Ref legal event code: PL

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: FR

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20030603

REG Reference to a national code

Ref country code: FR

Ref legal event code: ST