EP0054573B1 - Procédé de consolidation de produits fibreux à l'aide de dispersions de résine synthétique - Google Patents

Procédé de consolidation de produits fibreux à l'aide de dispersions de résine synthétique Download PDF

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Publication number
EP0054573B1
EP0054573B1 EP80108012A EP80108012A EP0054573B1 EP 0054573 B1 EP0054573 B1 EP 0054573B1 EP 80108012 A EP80108012 A EP 80108012A EP 80108012 A EP80108012 A EP 80108012A EP 0054573 B1 EP0054573 B1 EP 0054573B1
Authority
EP
European Patent Office
Prior art keywords
plastics
dispersion
weight
methacrylic acid
acrylic
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
EP80108012A
Other languages
German (de)
English (en)
Other versions
EP0054573A1 (fr
Inventor
Herbert Dr. Fink
Klaus Dr. Hübner
Egon Grumbach
Hans Ottofrickenstein
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.)
Roehm GmbH Darmstadt
Original Assignee
Roehm GmbH Darmstadt
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
Application filed by Roehm GmbH Darmstadt filed Critical Roehm GmbH Darmstadt
Priority to EP80108012A priority Critical patent/EP0054573B1/fr
Priority to DE8080108012T priority patent/DE3070134D1/de
Priority to AT80108012T priority patent/ATE11681T1/de
Publication of EP0054573A1 publication Critical patent/EP0054573A1/fr
Application granted granted Critical
Publication of EP0054573B1 publication Critical patent/EP0054573B1/fr
Expired legal-status Critical Current

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Classifications

    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
    • D04H1/58—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties by applying, incorporating or activating chemical or thermoplastic bonding agents, e.g. adhesives
    • D04H1/587—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties by applying, incorporating or activating chemical or thermoplastic bonding agents, e.g. adhesives characterised by the bonding agents used
    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
    • D04H1/58—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties by applying, incorporating or activating chemical or thermoplastic bonding agents, e.g. adhesives
    • D04H1/64—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties by applying, incorporating or activating chemical or thermoplastic bonding agents, e.g. adhesives the bonding agent being applied in wet state, e.g. chemical agents in dispersions or solutions

Definitions

  • the invention relates to a method for solidifying fiber structures by treatment with aqueous plastic dispersions.
  • the choice of the plastic dispersions to be used depends, among other things, on whether the finished fiber structure should be resistant to organic solvents. If this is not the case, plastic dispersions can be used which are free of formaldehyde-releasing substances and whose plastic content is essentially composed, for example, of alkyl esters of acrylic or methacrylic acid, vinyl esters and / or styrene and small amounts of ⁇ , ⁇ -unsaturated carboxylic acids.
  • plastic dispersions are used that can be crosslinked after coating or soaking and drying at elevated temperatures.
  • the crosslinking is achieved either by adding water-soluble aminoplast resins to the dispersions of the type mentioned above or by using plastic dispersions in the formation of which condensable formaldehyde derivatives, in particular N-methylolacrylamide or methacrylamide, are involved.
  • consolidated nonwovens are already known, for the manufacture of which plastic dispersions were used which are free of formaldehyde or of formaldehyde-releasing substances. They are produced with a content of 1 to 8 wt .-% units of an unsaturated carboxylic acid and subsequently neutralized with alkali. This does not significantly improve the sensitivity of the binder to solvents or plasticizers.
  • the invention has for its object to provide fiber structures with an equipment that is at least limited solvent-resistant or block-free or tack-free, and to do this use an aqueous plastic dispersion that is free of formaldehyde-releasing substances and whose plastic content consists predominantly of alkyl esters of acrylic or methacrylic acid, as well as small amounts of a, ⁇ -unsaturated carboxylic acids.
  • the stated object can be achieved with a plastic dispersion of this type, which can be added in the initial charge and under using the feed process using 1-4% by weight acrylic or / and methacrylic acid, based on the total weight of polymerizable compounds Addition of the other monomers has been prepared in the feed, the acrylic or methacrylic acid being used in the form of an alkali or ammonium salt.
  • the monomers as such or in the form of an aqueous emulsion are gradually run under polymerization conditions to a template in which the polymerization takes place.
  • the initial charge consists of an aqueous phase which generally contains a water-soluble polymerization initiator and one or more emulsifiers.
  • the improved solvent resistance of the coatings or impregnations produced in accordance with the invention depends on the fact that, in the preparation of the plastic dispersion to be used, acrylic or methacrylic acid in the form of its alkali metal or ammonium salt is dissolved in the initial charge.
  • Equivalent plastic dispersions cannot be prepared by gradually adding the acrylic or methacrylic acid or its salts together with the other monomers during the feed process or by adding the acrylic or methacrylic acid as such to the initial charge and only neutralizing it after the polymerization.
  • plastic dispersions which are free of formaldehyde-releasing substances by the process indicated above is known from OE-PS 236 643 and from FR-A-1 157 265.
  • the plastic dispersions produced in this way have not yet been used to solidify fiber structures.
  • the impregnations and coatings obtained would be characterized by improved resistance to organic solvents.
  • Plastic dispersions with a minimum film-forming temperature below 25 ° C. and with a Txmax value of the dispersed plastic (according to DIN 53445) below 50 ° C. are used with particular advantage for the process of the invention.
  • the plastic portion of the dispersion is preferably composed of more than 50% by weight of acrylic acid alkyl esters with 1-8 C atoms in the alkyl radical and for the most part predominantly from methacrylic acid alkyl esters with 1-4 C atoms in the alkyl radical.
  • Other water-insoluble monomers, such as. B. styrene, vinyl acetate or vinylidene chloride, can be involved in minor amounts in the construction of the plastic.
  • the share of Acrylic and / or methacrylic acid copolymerized in salt form is preferably 2-3% by weight calculated as free acid and based on the weight of the plastic.
  • the alkali salts are preferably the sodium and potassium salts.
  • the ammonium salts can be from ammonia or from organic amines, such as. B. ethanolamine.
  • the preferred method for producing the plastic dispersion is the emulsion feed method.
  • Part of the amount of water provided as the aqueous phase of the dispersion is placed in the polymerization vessel and the salt of acrylic and / or methacrylic acid is dissolved therein. be solved.
  • the initial charge is brought to a temperature suitable for carrying out the polymerization, preferably to about 50 to 80 ° C.
  • the monomers to be polymerized with the exception of acrylic or methacrylic acid, are emulsified, for which purpose a further amount of an emulsifier is expediently used.
  • the monomer emulsion is gradually run into the receiver over the course of several hours while the polymerization is taking place at the same time.
  • Additional polymerization initiators can be added continuously or in individual additions during the polymerization.
  • the amount of water and monomers are preferably matched to one another in such a way that a 40-60% dispersion is obtained.
  • the use of emulsifiers can optionally be dispensed with.
  • the monomers, apart from the acrylic acid or methacrylic acid salt, can also be added gradually in non-emulsified form. In this case, the entire water phase is added to the template at the beginning of the process.
  • the fiber structures that are consolidated according to the invention can consist of natural fibers, man-made fibers or of mixtures of different types of fibers.
  • the consolidation of mineral fiber structures, e.g. B. made of glass fibers or rock wool comes into consideration.
  • Flat fiber structures are essentially equipped; these include woven fabrics, knitted fabrics, non-woven fabrics, and papers, in particular absorbent base papers and cardboards.
  • the plastic dispersion can be applied as a coating on the surface of the fiber structure.
  • the fiber structure is preferably treated with the plastic dispersion in such a way that an impregnation that solidifies the entire cross section is achieved.
  • the amount of plastic dispersion used for solidification depends on the intended use of the solidified fiber structure.
  • a preferred application of the invention is the consolidation of light nonwovens with a basis weight of not more than 60 g / m2.
  • the dispersion can be applied to or introduced into the fiber structure by impregnation, spraying, splashing, brushing or printing. Depending on the application method used, the dispersion can be applied as a dilute liquor, for example with a binder content of 15 to 30% by weight, or as a thickened paste or as a foam. Conventional thickening agents, such as cellulose derivatives or water-soluble synthetic polymers, can be reacted in the pastes; the binder content is preferably 20 to 40% by weight.
  • the coated or impregnated fiber structure is dried. Conventional flat web dryers, cylinder dryers or screen drum dryers can be used for this.
  • the treated fiber structure is less prone to sticking to warm metal surfaces than products equipped with purely thermoplastic dispersions.
  • the so-called “binder tri wash loss”, abbreviated to BTV, is suitable, the determination of which is explained in more detail in the examples under IV. While the impregnation with dispersions which contain no carboxylate groups or in which the proportion of alkali metal carboxylate groups has not been incorporated in the manner described here gives BTV values of 80-100%, the binder loss in the fiber structures impregnated by the process of the invention results in reduced a fraction of that value. Even with an alkali methacrylate content of 1% (calculated as methacrylic acid, based on the plastic weight), a BTV value between 30 and 50% is achieved.
  • BKV Binder-Kochwasch-loss
  • the BKV value proves to a large extent depending on the drying temperature. After drying at room temperature, BKV values of up to 70% are observed. After drying or reheating at temperatures between 80 and 120 ° C - especially with a low carboxylate content - only binder losses of a few percent can be determined.
  • binder losses In the preferred range of 2-3% by weight carboxylate units, binder losses of between 4 and 10% by weight occur.
  • the binder losses depend on the type of fiber material and the plastic dispersion; the values mentioned here apply to a polyester fabric which was equipped with 50% by weight of a plastic dispersion composed of methyl methacrylate and butyl acrylate as the main components.
  • the mixture is stirred at 80 ° C. for one hour and then cooled to room temperature. A dispersion with a solids content of 45% is formed. To produce 50% dispersions, the water content is reduced accordingly.
  • Comparative dispersion C prepared in accordance with Example 10, but with the addition of methacrylic acid in the form of the free acid together with the monomer feed.
  • Comparative dispersion D prepared like comparative dispersion C, but neutralized the methacrylic acid units with the equivalent amount of KOH after completion of the polymerization.
  • Comparative dispersion E prepared as in Example 10, but gradual addition of the potassium methacrylate simultaneously with the addition of the other monomers.
  • a polyester fabric with a basis weight of 100 g / m 2 of polyester staple fibers is impregnated with a dispersion at room temperature and squeezed to a liquor absorption of 80 to 100% (based on the weight of the fabric) using a laboratory pad.
  • the moist fabric strip is dried in a tensioned state for 5 minutes at 120 ° C in a forced-air drying cabinet.
  • a sample measuring 18 x 18 cm is agitated with 125 ml of trichlorethylene at 20 ° C for 80 min, then rinsed with 100 ml of trichlorethylene and dried at 80 ° for 30 min. After storage for half an hour at room temperature, the sample is weighed out. The weight loss is determined in percent, based on the weight of the binder in the sample used.
  • a sample of 18 x 18cm size is 10 min at 90 ° with 125 ml of an aqueous wash liquor containing 3 g of Marseille soap and 2 g of calc. Soda contains, agitated, then rinsed once with hot water at 90 ° C and once with cold water and dried at 90 ° C for 30 min. 30 minutes after drying, the sample is weighed and the binder loss in percent, based on the weight of the binder in the sample used, is determined.
  • the comparative dispersions show that without neutralization of the carboxyl groups of the binder polymer (comparative dispersion C), very high binder losses occur in the tri-wash. These losses are significantly reduced by neutralization, while the losses in hot water only increase insignificantly despite the increased polarity of the binder. With subsequent neutralization (comparative dispersion D), particularly low binder losses are found, but the tests described under 111 indicate a high sensitivity of the film to plasticizers. With a uniform addition of the methacrylic acid salt (comparative dispersion E), the binder losses are higher than when used in the template according to the invention (example 10), but significantly lower than in the case of non-neutralized binder resin. In addition, the swelling in the plasticizer (see under 111) is unfavorably high.

Landscapes

  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Dispersion Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
  • Reinforced Plastic Materials (AREA)

Claims (8)

1. Procédé pour la consolidation de produits en fibres par traitement par des dispersions aqueuses de matière synthétiques qui sont dépourvues de substances glrnéràtrices d'aldéhyde formique et dont la partie matière synthétique est constituée principalement d'esters alcoyliques de l'acide acrylique ou méthacrylique, ainsi que de petites quantités d'acides carboxyliques α,β-insaturés, et par séchage consécutif, caractérisé en ce que le traitement est effectué avec une dispersion de matière synthétique pour la préparation de laquelle on charge préalablement une phase aqueuse qui contient en solution 1 à 4% en poids, par rapport au poids total des composés polymérisable entrant dans la constitution de la dispersion, d'acide acrylique et/ou méthacrylique sous la forme de leurs sels alcalins ou ammoniques, et on introduit peu à peu par écoulement, dans des conditions de polymérisation, les autres monomères, tels quels ou sous forme d'une émulsion aqueuse, dans la phase aqueuse, dans- laquelle a lieu la polymérisation.
2. Procédé selon la revendication 1, caractérisé en ce qu'on utilise une dispersion de matière synthétique contenant, par rapport à la teneur en matière synthétique, une proportion de 2 à 3% en poids de t'acide acrylique ou méthacrylique en liaison polymère sous la forme de sel.
3. Procédé selon la revendication 1 ou 2, caractérisé en ce qu'on utilise une dispersion de matière synthétique qui forme une pellicule aux alentours de 25°C et qui présente une valeur Tλmax de la matière synthétique dispersée inférieure à 50°C.
4. Procédé selon l'une quelconque des revendications 1 à 3, caractérisé en ce qu'on utilise une dispersion de matière synthétique qui est composée, pour plus de 50% en poids, par rapport à la partie matière synthétique, d'esters alcoyliques d'acide acrylique comportant 1 à 8 atomes de C dans le radical alcoyle et, pour le reste, principalement d'esters alcoyliques d'acide méthacrylique comportant 1 à 4 atomes de C dans le radical alcoyle.
5. Procédé selon l'une quelconque des revendications 1 à 4, caractérisé en ce que pour 100 parties en poids de fibres, on utilise au moins 10 parties en poids à sec de matière synthétique sous la forme de dispersion aqueuse de matière synthétique.
6. Procédé selon l'une quelconque des revendications 1 à 5, caractérisé en ce qu'on utilise, en thant que produits en fibres, des tissus et des nappes non tissées en fibres textiles ou du papier.
7. Procédé selon la revendication 6, caractérisé en ce qu'on utilise des nappes de fibres non tissées, ayant un poids par unité de surface qui ne dépasse pas 60 g/m2, pour le traitement de consolidation.
8. Procédé selon l'une quelconque des revendications 1 à 7, caractérisé en ce que les produits en fibres sont traités par la dispersion de matière synthétique par imprégnation, aspersion, enduction, placage ou impression.
EP80108012A 1980-12-18 1980-12-18 Procédé de consolidation de produits fibreux à l'aide de dispersions de résine synthétique Expired EP0054573B1 (fr)

Priority Applications (3)

Application Number Priority Date Filing Date Title
EP80108012A EP0054573B1 (fr) 1980-12-18 1980-12-18 Procédé de consolidation de produits fibreux à l'aide de dispersions de résine synthétique
DE8080108012T DE3070134D1 (en) 1980-12-18 1980-12-18 Process for the consolidation of fibrous material with dispersions of synthetic resin
AT80108012T ATE11681T1 (de) 1980-12-18 1980-12-18 Verfahren zum verfestigen von fasergebilden mit kunststoffdispersionen.

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
EP80108012A EP0054573B1 (fr) 1980-12-18 1980-12-18 Procédé de consolidation de produits fibreux à l'aide de dispersions de résine synthétique

Publications (2)

Publication Number Publication Date
EP0054573A1 EP0054573A1 (fr) 1982-06-30
EP0054573B1 true EP0054573B1 (fr) 1985-02-06

Family

ID=8186934

Family Applications (1)

Application Number Title Priority Date Filing Date
EP80108012A Expired EP0054573B1 (fr) 1980-12-18 1980-12-18 Procédé de consolidation de produits fibreux à l'aide de dispersions de résine synthétique

Country Status (3)

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EP (1) EP0054573B1 (fr)
AT (1) ATE11681T1 (fr)
DE (1) DE3070134D1 (fr)

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CA1144294A (fr) * 1978-12-04 1983-04-05 Walter G. De Witt, Iii Tissus lamelles non tisses convenant au revetement des couches

Also Published As

Publication number Publication date
DE3070134D1 (en) 1985-03-21
EP0054573A1 (fr) 1982-06-30
ATE11681T1 (de) 1985-02-15

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