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EP0041205B1 - Procédé pour la préparation de matériaux filtrants - Google Patents

Procédé pour la préparation de matériaux filtrants Download PDF

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Publication number
EP0041205B1
EP0041205B1 EP19810103970 EP81103970A EP0041205B1 EP 0041205 B1 EP0041205 B1 EP 0041205B1 EP 19810103970 EP19810103970 EP 19810103970 EP 81103970 A EP81103970 A EP 81103970A EP 0041205 B1 EP0041205 B1 EP 0041205B1
Authority
EP
European Patent Office
Prior art keywords
resin
paper
cellulose
monomer
paper web
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
EP19810103970
Other languages
German (de)
English (en)
Other versions
EP0041205A1 (fr
Inventor
Karl-Heinz Brodersen
Rolf Ing. Grad. Bade
Manfred Ing. grad. Römer
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.)
Md-Papierfabrik Pasing Nicolaus & Co
Morton Thiokol GmbH
Original Assignee
Md-Papierfabrik Pasing Nicolaus & Co
WIKOLIN POLYMER CHEMIE GmbH
Md-Papierfabrik Pasing Nicolaus & Co
Morton Thiokol GmbH
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 Md-Papierfabrik Pasing Nicolaus & Co, WIKOLIN POLYMER CHEMIE GmbH, Md-Papierfabrik Pasing Nicolaus & Co, Morton Thiokol GmbH filed Critical Md-Papierfabrik Pasing Nicolaus & Co
Publication of EP0041205A1 publication Critical patent/EP0041205A1/fr
Application granted granted Critical
Publication of EP0041205B1 publication Critical patent/EP0041205B1/fr
Expired legal-status Critical Current

Links

Classifications

    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
    • D21H17/03—Non-macromolecular organic compounds
    • D21H17/05—Non-macromolecular organic compounds containing elements other than carbon and hydrogen only
    • D21H17/18—Non-macromolecular organic compounds containing elements other than carbon and hydrogen only forming new compounds in situ, e.g. within the pulp or paper, by chemical reaction with itself, or other added substances, e.g. by grafting on the fibres
    • D21H17/19—Non-macromolecular organic compounds containing elements other than carbon and hydrogen only forming new compounds in situ, e.g. within the pulp or paper, by chemical reaction with itself, or other added substances, e.g. by grafting on the fibres by reactions only involving carbon-to-carbon unsaturated bonds
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H25/00—After-treatment of paper not provided for in groups D21H17/00 - D21H23/00
    • D21H25/04—Physical treatment, e.g. heating, irradiating
    • D21H25/06—Physical treatment, e.g. heating, irradiating of impregnated or coated paper
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H27/00—Special paper not otherwise provided for, e.g. made by multi-step processes
    • D21H27/08—Filter paper

Definitions

  • the invention relates to a method for producing filter materials for oil and air filters for internal combustion engines by impregnating a porous paper substrate based on cellulose with a dispersion of at least one resin and / or monomer curable by electron beams and subsequent curing with electron beams.
  • Filters are required for various technical purposes, which on the one hand should have a high retention capacity and on the other hand are resistant to the medium to be filtered.
  • filter papers with special impregnation are used.
  • the structure of this filter paper is such that on the one hand it opposes the passage of air due to innumerable pores, but on the other hand only allows the smallest and therefore harmless dust particles to pass through because of the fineness of the pores.
  • Filters with the same structure are also used as oil filters in internal combustion engines.
  • the filters were manufactured from porous paper webs that were impregnated with uncrosslinked phenolic resins.
  • the crosslinking or curing of the phenolic resins takes place after soaking at an elevated temperature.
  • This manufacturing process was very complex overall, since the resins were cured at temperatures in the order of 160 ° to 180 ° C. and with considerable residence times, so that curing systems of 30 to 50 meters in length are required.
  • the phenolic resin vapors released during the curing process have a considerable environmental impact.
  • the environmental protection problems essentially lie in the fact that the alcohol-soluble phenolic resins or phenolic resin vapors can reach the exhaust air or waste water.
  • the process was further complicated by the fact that the curing process could not be carried out in one process step, but had to be interrupted during the filter manufacture.
  • the hardening or condensation process was interrupted to allow the paper to be folded or pleated.
  • the final condensation was only carried out after the folding, in some cases with tears in the paper at the folded edges. This final condensation itself is necessary so that the paper no longer contains any volatile constituents that can migrate into the medium to be filtered.
  • the precondensation is carried out to such an extent that the paper or the resin contained therein no longer sticks to one another and can therefore be processed.
  • EP-A-24703 which represents an earlier right under Article 54 (3) and (4) EPC, has already proposed a method in which the impregnating agent is a solution or dispersion of a resin and / or monomers based on acrylic acid and / or methacrylic acid esters with polyols.
  • the impregnating agent is a solution or dispersion of a resin and / or monomers based on acrylic acid and / or methacrylic acid esters with polyols.
  • it is proposed to effect curing by electron radiation.
  • the phenolic resins are thus replaced by other resins, and the impregnated paper web is cured by electron radiation instead of the conventional heat curing in a drying channel.
  • the invention is therefore based on the object of specifying a method for producing filter materials for oil and air filters for internal combustion engines. These filter materials should be very economical to manufacture and enable high quality filters. The method is intended to avoid environmental pollution and to be able to be carried out with the lowest possible system expenditure.
  • the object is achieved in a method of the type mentioned in the invention in that the impregnation is carried out on a paper web in the paper machine with an aqueous emulsion with a resin and / or monomer content of 15 to 70 wt .-%, wherein the paper web consists of a predominantly long-fiber cellulose with a low freeness of 13 to 15 Schopper-Riegler.
  • the paper machine which is anyway necessary for producing the paper web, and an installation for electronic radiation curing, the paper machine being provided at a suitable point with a device which permits impregnation of the paper web.
  • the impregnation can be done through a commission, e.g. B. a size press can be performed.
  • An aqueous emulsion of an electronically curable resin is used as the impregnating agent.
  • FR-A-2 241 384 has also made known a process for the production of impregnated papers, in which the impregnation can take place in the paper machine.
  • the curing can then be carried out using electron beams.
  • This process is also not concerned with the production of porous paper for further processing into filters for internal combustion engines. Rather, the aim is to improve the wet strength of the paper, while still obtaining papers which have a relatively high water absorption capacity.
  • the papers obtained in this way have good air permeability, but also a relatively high absorption capacity for water, which makes them unsuitable as filter papers for motor vehicle purposes.
  • FR-A-1 359 241 a process for the production of impregnated papers is known, the paper machine being subjected to an impregnation with an aqueous emulsion of at least one resin and / or monomer that can be hardened by high-energy radiation in the paper machine and the impregnated paper web is then subjected to curing by means of ⁇ -rays.
  • the manufactured product replaces certain fabrics and contains long fibers.
  • the production of filter paper is not addressed.
  • the resin to be used in the process according to the invention is added to the paper web in the paper machine in the form of an aqueous emulsion.
  • Resins and / or monomers based on acrylic acid and / or methacrylic acid esters with polyols are used.
  • the emulsion itself has a resin content of 15 to 70% by weight.
  • the use of an emulsion has the advantage that the resin particles can penetrate the paper very well.
  • the resin is attached to the paper in an amount of 10 to 30% by weight, preferably 20% by weight.
  • the distribution of the resin should be even, so that the filter effect is even across the entire filter.
  • the preferred resin content in the paper for the filters is 20% by weight.
  • the resin content should be as low as possible.
  • the resin content can vary depending on the intended use of the filter material and the specified values such as burst pressure, rigidity of the filter, etc. With high strengths, a higher resin content of up to 30% is introduced, while with low strengths a resin content of up to 10% is sufficient. These statements also apply to papers for other areas of use. With a view to safe operation, no solvents should be used that could cause an explosion.
  • the resin components are fully cross-linked in the electron beam curing system. This is very important, as any non-cross-linked portions, as noted above, can be absorbed by the filtered medium.
  • the content of soluble components in the finished filter should be as low as possible.
  • the production according to the invention has the advantage that the resins used are not soluble in alcohols.
  • the alcohols can lead to the dissolution of conventional resins.
  • alcohol fuels can also remove uncondensed phenolic resin from the filters.
  • the paper web is made from a predominantly long-fiber cellulose.
  • the proportion of long-fiber cellulose is preferably more than 90%. It is also favorable to use a cotton cellulose as cellulose.
  • the cellulose used has a low freeness of 13 to 15 Schopper-Regier. Due to the low degree of grinding of the cellulose used, which, as already mentioned above, is preferably cotton cellulose, a so-called cotton linter, the paper web and also the subsequent filter are given high strength. In order to increase the strength of the paper web, customary so-called wet-strength agents can also be added to the pulp.
  • the resin uptake by the paper web is preferably controlled via the initial moisture of the paper web when it enters the size press.
  • the speed of the paper web is used to control the resin uptake. At higher paper web speeds, smaller amounts of resin are taken up.
  • the paper web After radiation curing, the paper web is cut into individual sheets corresponding to the filter sizes. These sheets are folded, provided with an adhesive line on one edge and glued together. It should be noted that the porosity of the filter papers produced in this way is very remarkable. The less resin is used, the better the filter effect. However, the burst pressure is all the less. Depending on the purpose for which the filter is used, more or less resin can consequently be added to the paper web, i. that is, the strength of the paper web can be increased more or less.
  • the paper webs produced according to the invention can be subjected to folding without damage occurring in the paper web at the folded edges. Consequently, the folded air filters required for internal combustion engines can be produced particularly well from the paper web.
  • the filters produced in this way also have a number of other advantages; hold like that the filters put out a high pressure.
  • a burst pressure of 2.2 to 2.5 bar is required.
  • the lower limit is generally considered to be 1.8 bar.
  • Filters manufactured using the new process have burst pressures that are significantly higher.
  • the filters previously produced from phenol generally had a brown color
  • the filters produced by the method according to the invention have no coloration due to the method, i. that is, the filters are white. This is very cheap, for example, if the color alone is used to determine whether the filter was already in use or not.
  • aqueous emulsions of monomers or resins which can be hardened by electron radiation or other high-energy radiation are used as impregnation agents.
  • Particularly suitable monomers are polyacrylated and / or polymethacrylated polyols, polyacrylated polyols being preferred because of the higher reaction rate.
  • Suitable resins for preparing the emulsions are, for example, the resins and / or monomers proposed in the aforementioned EP-A-24703.
  • hydroxyl groups of the polyols mentioned can be wholly or partially esterified by acrylic acid and / or methacrylic acid.
  • Specific examples of the present invention usable monomers are trimethylolpropane triacrylate, hexanediol diacrylate, pentaerythritol tetraacrylate, pentaerythritol triacrylate, hexane-1, 6-diol diacrylate, Diäthylenglykoldiacrylat, Triäthylenglykoldiacrylat, Tetraäthylenglykoldiacrylat, tripropylene glycol diacrylate, 2-Hydroxäthylacrylat, 2-Hydroxypropoylacrylat, Hexandiolmonoacrylate and butandiolmonoacrylate and the corresponding methacrylates or mixed acrylate Methacrylates.
  • the monomers can be used alone or in a mixture, if appropriate with high or low molecular weight prepolymers.
  • Particularly suitable monomers are pentaerythritol triacrylate or pentaerythritol acrylate mixtures with an average degree of esterification of 3 to 3.3 and with a viscosity of 600-1 200 mPa.s (measured at 20 ° C. with the Brookfield viscometer, type RVT).
  • High or low molecular weight resins or oligomers are suitable as resins.
  • these are soluble polyurethane acrylates formed from the aforementioned hydroxy-functional acrylate monomers.
  • the molecular weight of such resins or oligomers is preferably in the range from 800-8,000 and their viscosities go from 1,000-50,000 mPa.s.
  • the content of acrylic and / or methacrylic unsaturated monomer units is, for example, 2-6 per molecule.
  • Resins of this type are produced by customary procedures, for example as described in DE-OS-2 530 896 and DE-OS-2 542 314.
  • a polyol is reacted with a di-isocyanate.
  • the content of free NCO groups reached is then saturated with hydroxy-functional acrylate or methacrylate monomers.
  • the person skilled in the art can choose amounts and reaction conditions such that the desired molecular weights and the desired content of acrylic and / or methacrylic unsaturated monomer units are achieved.
  • the viscosities can be varied, for example, by appropriate dilution of the resins with monomers.
  • the acrylic or methacrylic, unsaturated monomers and / or oligomers explained above on the basis of examples are processed into oil-in-water (O / W) emulsions using emulsifiers.
  • the total solids content of these emulsions which mainly consists of the monomer and / or oligomer together with the emulsifiers, is 15 to 70% by weight, preferably 20 to 60% by weight and in particular approximately 40% by weight, based on the finished emulsion.
  • the particle size of the resulting emulsion is ⁇ 1 ⁇ m and preferably 0.4 to 0.6 ⁇ m. This particle size is achieved by conventional measures, such as the selection of suitable emulsifiers and emulsification conditions.
  • Suitable emulsifiers for the emulsions used according to the invention are in principle nonionic emulsifiers, anionic and cationic emulsifiers, alone or in a mixture with one another.
  • emulsions with a particle size of ⁇ 1 ⁇ , m and a heat storage stability of 2 to 6 months at temperatures of 30 to 60 ° C were produced.
  • the amount of emulsifier used depends on the monomers and / or oligomers used and on the emulsifying conditions. In general, 1 to 7% by weight, preferably 1 to 3% by weight, of the emulsifiers or mixtures thereof, calculated on the inner phase or the total solids content of the OIW emulsion, is required.
  • Amounts of 0.02-0.4% by weight have proven successful, but particularly amounts of 0.1-0.3% by weight, based on the total batch, have proven successful.
  • the amount used is preferably 0.05-0.5% by weight, based on the total batch, in particular 0.1-0.4% by weight.
  • the aqueous emulsions used according to the invention have a solids content (monomer and / or oligomer plus emulsifier and further additives or auxiliaries) of 15 to 70% by weight.
  • concentration of the monomer and / or oligomer or resin ultimately depends on the desired degree of coverage of the substrate with the monomer, oligomer or resin.
  • the fleece or paper materials impregnated according to the invention are hardened by electron radiation, as mentioned at the beginning.
  • the unsaturated acrylate resin is cured by radial chain polymerization, which leads to ketene growth with a high three-dimensional degree of branching.
  • Electron or beta radiation is used.
  • the radiation can be generated by conventional electron sources.
  • one or more stage electron accelerators are used, for example the electron accelerators described in EP-A-24703.
  • the paper webs impregnated according to the invention are optionally passed under an inert gas, such as nitrogen, past a window from which the electron radiation emerges.
  • the acceleration voltages of the single-stage or multi-stage electron accelerators used are, for example, about 150 to 500 kV, the radiation dose is, for example, about 0.1 to about 16 Mrad.
  • the flask is equipped with a condenser (water-cooled), an agitator with a patent plug, which allows the flask to be covered with nitrogen during the manufacturing process (because of the NCO / water reaction), as well as a thermometer for temperature control.
  • NCO target 6.24 ⁇ 0.1%.
  • NCO target 0.00%
  • item 4 is added and mixed thoroughly. After mixing, the reactor contents are cooled to approx. 40 ° C and the resin is filled.
  • a paper web is made from a cellulose with a long fiber content of 80% in a paper machine.
  • an aqueous emulsion according to Example 3 with a monomer content of 30% is filled into the size press of the paper machine.
  • the paper web is passed through the size press and impregnated.
  • an electron radiation curing system is set up, through which the paper web is passed.
  • the result is an impregnated paper that has a resin content of 21% and is porous with high strength.
  • the burst pressure is over 3 atmospheres.
  • the resin is fully cured.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Paper (AREA)

Claims (6)

1. Procédé de fabrication de matériaux pour filtres, destinés à des filtres à huile et à air de moteurs à combustion interne, par imprégnation d'un substrat de papier poreux à base de cellulose avec une dispersion d'au moins une résine et/ou d'un monomère durcissables par un rayonnement d'électrons suivie d'un durcissement par un rayonnement d'électrons, caractérisé en ce que l'imprégnation sur la bande de papier dans la machine à papier s'effectue avec une émulsion aqueuse dans laquelle la proportion en poids de résine et/ou de monomère est de 15 à 70 %, la bande de papier étant constituée en majeure partie par une cellulose fibreuse qui présente un taux de broyage faible de 13 à 15 Schopper-Riegler.
2. Procédé selon la revendication 1, caractérisé en ce que des émulsions aqueuses de résine et/ou de monomères à base d'esters d'acide acrylique et/ou d'acide méthacrylique sont utilisées avec des polyols.
3. Procédé selon l'une des revendications 1 ou 2, caractérisé en ce que la résine et/ou le monomère est appliqué en couche sur le papier dans une proportion de 10 à 30 % en poids, de préférence de 20 %.
4. Procédé selon l'une des revendications 1 à 3, caractérisé en ce que la proportion de cellulose à longues fibres dépasse 90 %.
5. Procédé selon l'une des revendications 1 à 4, caractérisé en ce que la cellulose est de la çellulose de coton.
6. Procédé selon l'une des revendications 1 à 5, caractérisé en ce que la bande de papier est, après le durcissement par irradiation, découpée en feuilles correspondant aux dimensions du filtre et en ce que les diférentes feuilles sont pliées, munies d'un adhésif sur l'un de leurs bords et collées.
EP19810103970 1980-05-29 1981-05-23 Procédé pour la préparation de matériaux filtrants Expired EP0041205B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE19803020333 DE3020333C2 (de) 1980-05-29 1980-05-29 Verfahren zur Herstellung von porösem Papier
DE3020333 1980-05-29

Publications (2)

Publication Number Publication Date
EP0041205A1 EP0041205A1 (fr) 1981-12-09
EP0041205B1 true EP0041205B1 (fr) 1985-12-11

Family

ID=6103466

Family Applications (1)

Application Number Title Priority Date Filing Date
EP19810103970 Expired EP0041205B1 (fr) 1980-05-29 1981-05-23 Procédé pour la préparation de matériaux filtrants

Country Status (4)

Country Link
EP (1) EP0041205B1 (fr)
BR (1) BR8103343A (fr)
DE (1) DE3020333C2 (fr)
FI (1) FI68436C (fr)

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE4114281C2 (de) * 1991-05-02 1996-05-02 Hoelter Heinz Verfahren zur Herstellung eines Chemisorptionsfilters und Vorrichtung zur Durchführung eines derartigen Verfahrens
DE102005032395A1 (de) * 2005-07-12 2007-01-25 Mahle International Gmbh Filtermedium für technische Anwendungen und Verfahren seiner Herstellung

Family Cites Families (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB794183A (en) * 1954-03-01 1958-04-30 Wipac Dev Ltd Improvements in and relating to resin-impregnated filter paper
FR1359241A (fr) * 1963-03-12 1964-04-24 Papiers imprégnés ou en duits à grande vitesse de production
FR2241384B1 (fr) * 1973-05-30 1976-06-11 Commissariat Energie Atomique
SE417849B (sv) * 1974-11-20 1981-04-13 Billingsfors Bruks Ab Forfarande for tillverkning av impregnerad och ytbehandlad folie
BE847418A (fr) * 1975-12-11 1977-02-14 Procede pour rendre transparentes des feuilles de matiere fibreuse et produits obtenus,
DE2933998C2 (de) * 1979-08-22 1987-05-27 Otto Dürr Anlagenbau GmbH, 7000 Stuttgart Verfahren und Vorrichtung zur Herstellung eines imprägnierten Papier- oder Vliessubstrats

Also Published As

Publication number Publication date
DE3020333A1 (de) 1981-12-10
DE3020333C2 (de) 1983-12-29
BR8103343A (pt) 1982-02-16
FI68436B (fi) 1985-05-31
FI811664L (fi) 1981-11-30
EP0041205A1 (fr) 1981-12-09
FI68436C (fi) 1985-09-10

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