EP0207366B1 - Procédé de filtration de bains de nettoyage à sec et adjuvants utilisés sous forme de silicates en couches préparés - Google Patents

Procédé de filtration de bains de nettoyage à sec et adjuvants utilisés sous forme de silicates en couches préparés Download PDF

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Publication number
EP0207366B1
EP0207366B1 EP86108285A EP86108285A EP0207366B1 EP 0207366 B1 EP0207366 B1 EP 0207366B1 EP 86108285 A EP86108285 A EP 86108285A EP 86108285 A EP86108285 A EP 86108285A EP 0207366 B1 EP0207366 B1 EP 0207366B1
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Prior art keywords
cleaning
filtration
layer
prepared
silicate
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EP86108285A
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German (de)
English (en)
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EP0207366A3 (en
EP0207366A2 (fr
Inventor
Werner Grünewälder
Margarete Schäfer
Winfried Dr. Wichelhaus
Wolfgang Dr. Von Rybinski
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Henkel AG and Co KGaA
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Henkel AG and Co KGaA
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Classifications

    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06L—DRY-CLEANING, WASHING OR BLEACHING FIBRES, FILAMENTS, THREADS, YARNS, FABRICS, FEATHERS OR MADE-UP FIBROUS GOODS; BLEACHING LEATHER OR FURS
    • D06L1/00—Dry-cleaning or washing fibres, filaments, threads, yarns, fabrics, feathers or made-up fibrous goods
    • D06L1/02—Dry-cleaning or washing fibres, filaments, threads, yarns, fabrics, feathers or made-up fibrous goods using organic solvents
    • D06L1/10—Regeneration of used chemical baths

Definitions

  • the invention relates to a method for the filtration of organic solvent-containing liquors in dry cleaning. It also concerns filter aids used in the filtration of these fleets.
  • filter cartridges are used for the filtration of the soiled cleaning liquors, the filtration result is significantly better.
  • the cartridges of such filters contain activated carbon or mixtures of activated carbon and activated alumina (bentonite). Such substances not only have an exceptionally large surface area, but also show a good adsorption effect against loosened soiling. The cleaning liquors filtered with it are therefore significantly cleaner than those filtered through diatomaceous earth filters, so that the time of a subsequent distillation of the cleaning liquors can be delayed.
  • Cartridge filters of this type are described, for example, in the current FCR information no. 174 of the Chemical Cleaning Research Center, published in July 1977.
  • a disadvantage of such adsorption filters is the surfactant content of certain cleaning liquors.
  • Such surfactants which originate, for example, from the predetach, are insufficiently adsorbed. This leads to an accumulation of pre-detaching agents and cleaning boosters in the cleaning liquors.
  • the invention has for its object to largely free the solvents or solvent mixtures used in chemical cleaning by improved filtration of dissolved contaminants, odors and dyes, pre-detaching agents and cleaning boosters, so that distillation of the solvent is only necessary at large intervals.
  • the invention therefore relates to a process for the filtration of organic solvent-containing liquors in dry cleaning using silicate filter aids, which is characterized in that natural and / or synthetic sheet silicates with an exchange capacity for cations not less than 30 meq / 100 g sheet silicate with or several ammonium compounds of the general formula (I) in which R 1 , R 2 , R 3 and R 4 represent hydrogen, alkyl or alkenyl groups or two or three of the radicals R 1 to R 4 , including the nitrogen atom, can be closed to form an aliphatic or aromatic heterocyclic ring system, where the respective Alkyl or alkenyl groups can be branched or unbranched and can contain cycloalkyl groups, aryl groups, ether bonds, amine bonds, amide bonds and ester bonds and can be substituted by hydroxyl groups or halide and have a number of C atoms in the range from 1 to 18 and the total number of C -Atoms in the cation is above 12 and
  • the invention also relates to filter aids for use in the filtration of cleaning liquors from dry cleaning, which are characterized in that they are mixed with ammonium compounds of the above general formula (I) in an amount of 2 to 60% by weight, based on the total weight of the modified Layered silicates, prepared natural and / or synthetic layered silicates in combination with diatomaceous earth and / or activated carbon.
  • silicate materials of natural and / or synthetic origin are suitable as layer silicates.
  • mica-like sheet silicates with a three-layer structure from the group of the smectites are used, but vermiculite and the sodium phyllosilicates, which belong to the non-mica-like sheet silicates, are also suitable.
  • the smectites include montmorillonite, saponite, beidellite and hectorite; Examples of phyllosilicates are kenyaite, magadiite, makatite and kanemite.
  • Bentonites with a high content of montmorillonite or hectorite are preferably used, natural bentonites in untreated form or, if appropriate, in one with acids or alkalis for cleaning and removing interfering cations are used in a manner known per se pretreated.
  • the most important parameter of the layered silicate materials that can be used is their exchange capacity for cations. According to the invention, this size should not be less than 30 meq / 100 g of layered silicate. Smectite clay minerals whose cation exchange capacity is between 50 and 120 meq / 100 g of layered silicate are particularly preferred.
  • Natural and / or synthetic phyllosilicates with the above-mentioned properties are mixed according to methods known per se with one or more long-chain ammonium compounds of the above-mentioned general formula (I) in an amount of 2 to 60% by weight, based on the total weight of the modified phyllosilicate. prepared. This can be done, for example, by treating the corresponding silicates with solutions of the desired ammonium compounds and thereby achieving an exchange of alkali metal cations of the layered silicates for the ammonium cations.
  • the layered silicates are preferably prepared with amounts of ammonium compounds in the range from 5 to 30% by weight, particularly preferably in the range from 10 to 25% by weight.
  • the quaternary ammonium compounds are particularly preferred; that is, compounds in which none of the radicals R 1 to R 4 is hydrogen.
  • the anion X - stands for anions of water-soluble acids with a dissociation constant above 10-5 , preferably for chloride, bromide, acetate, hydrogen sulfate or hydrogen phosphate, but especially for chloride.
  • Lauryltrimethylammonium chloride and distearyldimethylammonium chloride have proven particularly useful for the preparation of natural and / or synthetic layered silicates.
  • other quaternary ammonium sets for example containing aromatic radicals R, can also be used with advantage, such as, for example, cetyldimethylbenzylammonium chloride.
  • Laurylpyridinium chloride is mentioned as an example of quaternary ammonium salts of the general formula (I), in which the organic radicals R, including the nitrogen atom, can be closed to form a heterocyclic ring system.
  • the natural and / or synthetic layered silicates prepared with the ammonium compounds mentioned are used in the process according to the invention as feed for precoat or cartridge filters, cartridge filters being particularly preferred.
  • the feed can either consist exclusively of the prepared layered silicates mentioned or, preferably, contain admixtures of conventional further filter aids, for example diatomaceous earth and / or activated carbon. If mixtures of diatomaceous earth / layered silicate or activated carbon / layered silicate are used, the mixing ratio of the components mentioned is 80:20 to 50:50, particularly preferably 70:30 to 50:50.
  • the filter aids described are much more suitable for use in the process according to the invention for the filtration of liquors containing organic solvents in chemical cleaning than conventional adsorption filters which contain kieselguhr, activated carbon, zeolites or mixtures of these materials.
  • the use of the filter aids mentioned has great advantages, in particular if trichlorethylene, 1,1,1-trichloroethane, perchlorethylene, monofluorotrichloromethane, trifluorotrichloroethane or mixtures of the solvents mentioned are present as contaminated solvents in the cleaning liquors.
  • the cleaning liquors can be almost completely freed from loosened dirt, odors and dyes, pre-detachment agents and cleaning enhancers.
  • the distillation of the solvents which is often required according to conventional filtration processes, is only required much less frequently. This not only saves solvents, but also significantly reduces energy costs.
  • the filter aids which consist of a mixture of layered silicate with diatomaceous earth or activated carbon, are always characterized by particularly universal cleaning properties.
  • Example 1 As a comparison of Example 1 and Comparative Example 1 shows, the fatty acid content and the solids content of the cleaning liquor could be greatly reduced when the layered silicate loaded, the cleaning booster could even be completely removed from the liquor.
  • the unloaded layered silicate showed worse results in all three cases.
  • Example 2 shows that the filtration with the prepared layered silicate led to significantly better filtration results; the amount of dissolved impurities was only a fraction of the impurities after filtration with unprepared layered silicate.
  • Example 3 Under the conditions described in Example 3, a precoat filter was used, which was charged with 70 g of diatomaceous earth and 30 g of powdered activated carbon. The results are shown in Table 1.
  • a cleaning test liquor was prepared which contained trichlorethylene as the organic solvent, to which 10 g of tallow fatty acid were added per liter of organic solvent.
  • the solvent was also colored strongly red by peeling off a textile naphthol color. It was pumped in circulation for two hours through a filter which was charged exclusively with a hectorite which contained lauryltrimethylammonium chloride as a quaternary ammonium compound in an amount of 5% by weight. After the filtration, samples were taken from the test liquor and examined for their fatty acid content and their color behavior. The results are shown in Table 3 below.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Detergent Compositions (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
  • Filtration Of Liquid (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Silicates, Zeolites, And Molecular Sieves (AREA)

Claims (10)

1. Procédé de filtration des bains contenant des solvants organiques dans le nettoyage à sec, en utilisant des adjuvants de filtration silicatiques, caractérisé en ce que
(a) l'on prépare des silicates naturels et/ou synthétiques stratifiés possédant une capacité échangeuse de cations non inférieure à 30 meq/100 g de silicate stratifié avec un ou plusieurs composés ammonium de la formule générale (I)
Figure imgb0009
dans laquelle R1, R2, R3 et R4 présentent l'hydrogène, des groupements alkyle ou alcényle ou dans laquelle deux ou trois des résidus R à R4, y compris l'atome d'azote peuvent être fermés en une combinaison cyclique aliphatique ou aromatique hétérocyclique, dans laquelle les groupements alkyle ou alcényle respectifs peuvent être ramifiés ou non ramifiés et renfermer des groupements cycloalkyle et aryle, des liaisons éther, amine, amide et ester, peuvent être substitués par des groupements hydroxyle ou halogéno et comportent un nombre d'atomes de carbone compris dans l'intervalle de 1 à 18, le nombre total d'atomes de carbones dans le cation étant supérieur à 12, et dans laquelle X` représente des anions d'acides hydrosolubles dont la constante de dissociation est supérieure à 10 , dans une proportion de 2 à 60 % en poids par rapport au poids total du silicate stratifié modifié; en ce que
(b) l'on charge un filtre à couche ou à cartouche de silicates stratifiés préparés selon l'étape (a), seuls ou en association avec de la diatomite et/ou du charbon actif, et en ce que
(c) l'on fait transiter par le filtre préparé des mélanges de solvants utilisés dans le nettoyage à sec.
2. Procédé selon la revendication 1, caractérisé en ce que l'on utilise des silicates stratifiés micaciques à triple couche du groupe de la smectite.
3. Procédé selon la revendication 1 ou 2, caractérisé en ce que l'on utilise de la bentonite à teneur élevée en montmorillonite.
4. Procédé selon la revendication 1 ou 2, caractérisé en ce que l'on utilise de la bentonite à teneur élevée en hectorite.
5. Procédé selon les revendications 1 à 4, caractérisé en ce que l'on utilise des minéraux de smectite dont la capacité échangeuse de cations est comprise dans l'intervalle de 50 à 120 meq/100 g de silicate stratifié.
6. Procédé selon les revendications 1 à 5, caractérisé en ce que l'on utilise des silicates stratifiés qui sont préparés avec 5 à 30 % en poids, en particulier de préférence avec 10 à 25 % en poids d'un composé ammonium de la formule générale (I).
7. Procédé selon les revendications 1 à 6, caractérisé en ce que l'on utilise pour la préparation des silicates stratifiés des composés ammonium quaternaire de la formule générale (1), dont les résidus R1 à R4 présentent un nombre total d'atomes de carbone compris dans l'intervalle de 14 à 38.
8. Procédé selon les revendications 1 à 7, caractérisé en ce que l'on utilise en tant que sels d'ammonium quaternaire des composés de la formule générale (I), dans laquelle au moins deux résidus R représentent chacun un résidu alkyle comportant 1 à 3 atomes de carbone, un ou deux résidus R représentent un résidu alkyle comportant 9 à 18 atomes de carbone et X- représente un chlorure, en particulier de préférence un chlorure de triméthylammonium laurique ou un chlorure de diméthylammonium distéarylique.
9. Procédé selon les revendications 1 à 3, caractérisé en ce que l'on utilise des filtres qui sont chargés de mélanges de diatomite et de silicate stratifié ou de charbon actif et de silicate stratifié, dans un rapport de mélange compris dans l'intervalle de 80 : 20 à 50 : 50, de préférence dans l'intervalle de 70 : 30 à 50 : 50.
10. Adjuvants de filtration pour utilisation dans la filtration des bains de nettoyage à sec, caractérisés en ce qu'ils comprennent des silicates naturels et/ou synthétiques stratifiés possédant une capacité échangeuse de cations non inférieure à 30 meq/100 g de silicate stratifié en association avec de la diatomite et/ou du charbon actif, préparés avec des composés ammonium de la formule générale (I)
Figure imgb0010
dans laquelle R1, R2, R3 et R4 représentent l'hydrogène, des groupements alkyle ou alcényle ou dans laquelle deux ou trois des résidus R1 à R4, y compris l'atome d'azote peuvent être fermés en une combinaison aliphatique ou aromatique hétérocyclique, dans laquelle les groupements alkyle ou alcényle respectifs peuvent être ramifiés ou non ramifiés et renfermer des groupements cycloalkyle, aryle, des liaisons éther, amine, amide et ester, peuvent être substitués par des groupements hydroxyle ou halogéno et comportent un nombre d'atomes de carbone compris dans l'intervalle de 1 à 18, le nombre total d'atomes de carbones dans le cation étant supérieur à 12, et dans laquelle X- représente des anions, dans une proportion de 2 à 60 % en poids par rapport au poids total du silicate stratifié modifié, en association avec de la diatomite et/ou du charbon actif.
EP86108285A 1985-06-27 1986-06-18 Procédé de filtration de bains de nettoyage à sec et adjuvants utilisés sous forme de silicates en couches préparés Expired EP0207366B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE3522932 1985-06-27
DE19853522932 DE3522932A1 (de) 1985-06-27 1985-06-27 Verfahren zur filtration von flotten in der chemischreinigung und dabei verwendete filterhilfsmittel in form praeparierter schichtsilikate

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EP0207366A2 EP0207366A2 (fr) 1987-01-07
EP0207366A3 EP0207366A3 (en) 1987-05-06
EP0207366B1 true EP0207366B1 (fr) 1989-12-06

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EP86108285A Expired EP0207366B1 (fr) 1985-06-27 1986-06-18 Procédé de filtration de bains de nettoyage à sec et adjuvants utilisés sous forme de silicates en couches préparés

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US (1) US4774004A (fr)
EP (1) EP0207366B1 (fr)
JP (1) JPS626970A (fr)
DE (2) DE3522932A1 (fr)
ES (1) ES2000054A6 (fr)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE3710849A1 (de) * 1987-04-01 1988-10-20 Henkel Kgaa Verwendung von mit quartaeren ammoniumverbindungen beladenen schichtsilikaten als seifhilfsmittel in seifprozessen zum fixieren von farbstoffen
JP3708542B2 (ja) * 1993-08-13 2005-10-19 ミネソタ マイニング アンド マニュファクチャリング カンパニー その上に不溶性酵素粒子を含有するカートリッジ・フィルター
US5468847A (en) * 1994-03-10 1995-11-21 Minnesota Mining And Manufacturing Company Method of isolating and purifying a biomacromolecule
US6027651A (en) * 1994-06-06 2000-02-22 Cash; Alan B. Process for regenerating spent solvent
US5785861A (en) * 1995-03-13 1998-07-28 Dufresne; Peter Regeneration of perchloroethylene
US5674389A (en) * 1996-01-29 1997-10-07 Rhee; Choong H. Removal of tetrachloroethylene impurity from water
AR036452A1 (es) * 2001-09-10 2004-09-08 Procter & Gamble Filtro para remocion de contaminantes de un fluido lipofilo, proceso para remover contaminante y fluido filtrado por dicho proceso
US7276162B2 (en) * 2001-09-10 2007-10-02 The Procter & Gamble Co. Removal of contaminants from a lipophilic fluid
JP5085954B2 (ja) * 2007-02-23 2012-11-28 スリーエム イノベイティブ プロパティズ カンパニー フッ素系溶剤含有溶液の精製方法及び精製装置ならびに洗浄装置
EP2123822A1 (fr) * 2008-05-14 2009-11-25 Süd-Chemie Ag Utilisation d'adsorbants pour la purification de solvants de nettoyage à sec

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Publication number Priority date Publication date Assignee Title
US3368678A (en) * 1965-01-11 1968-02-13 Dow Chemical Co Purification of dry cleaning solvents
DE3007633A1 (de) * 1980-02-29 1981-09-10 Henkel KGaA, 4000 Düsseldorf Verfahren zur aufbereitung von chlorierten kohlenwasserstoffen in der chemischreinigung
US4386010A (en) * 1980-09-02 1983-05-31 Engelhard Corporation Treated attapulgite clay composition
DE3274954D1 (en) * 1981-09-30 1987-02-12 Radecca Inc Method of immobilizing organic contaminants and non-flowable matrix produced therefrom

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Publication number Publication date
DE3667309D1 (de) 1990-01-11
EP0207366A3 (en) 1987-05-06
ES2000054A6 (es) 1987-11-16
US4774004A (en) 1988-09-27
DE3522932A1 (de) 1987-01-08
JPS626970A (ja) 1987-01-13
EP0207366A2 (fr) 1987-01-07

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