WO2025008068A1 - Dispersion d'électrofilage et procédé de production d'un non-tissé d'élastomère de silicone électrofilé - Google Patents

Dispersion d'électrofilage et procédé de production d'un non-tissé d'élastomère de silicone électrofilé Download PDF

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WO2025008068A1
WO2025008068A1 PCT/EP2023/068662 EP2023068662W WO2025008068A1 WO 2025008068 A1 WO2025008068 A1 WO 2025008068A1 EP 2023068662 W EP2023068662 W EP 2023068662W WO 2025008068 A1 WO2025008068 A1 WO 2025008068A1
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electrospinning
dispersion
radicals
crosslinking
silicone
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German (de)
English (en)
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Sabin-Lucian Suraru
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Wacker Chemie AG
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Wacker Chemie AG
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    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00—Formation of filaments, threads, or the like
    • D01D5/0007—Electro-spinning
    • D01D5/0015—Electro-spinning characterised by the initial state of the material
    • D01D5/003—Electro-spinning characterised by the initial state of the material the material being a polymer solution or dispersion
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00—Use of organic ingredients
    • C08K5/04—Oxygen-containing compounds
    • C08K5/14—Peroxides
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
    • C08L83/04—Polysiloxanes
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D1/00—Treatment of filament-forming or like material
    • D01D1/02—Preparation of spinning solutions
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00—General methods for the manufacture of artificial filaments or the like
    • D01F1/02—Addition of substances to the spinning solution or to the melt
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/58—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products
    • D01F6/76—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from other polycondensation products
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
    • C08G77/04—Polysiloxanes
    • C08G77/12—Polysiloxanes containing silicon bound to hydrogen
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
    • C08G77/04—Polysiloxanes
    • C08G77/20—Polysiloxanes containing silicon bound to unsaturated aliphatic groups

Definitions

  • the present invention relates to a silicone elastomer-based electrospinning solution and its use for producing nonwovens by means of an improved electrospinning process.
  • Electrospinning is a process known in the art for producing nonwovens with controllable fiber diameters of a few micrometers to a few nanometers.
  • a polymer melt, solution or dispersion is spun in a strong electric field (approx. 10 - 50 kV) between the spinneret (capillary) and the collector to form a sub-micrometer-thin fiber and is then deposited on a substrate as a nonwoven.
  • the throughput of the method can be achieved by simply numbering up the nozzles. Details of the electrospinning process are described, for example, in A. Greiner et al. Angew. Chem. 2007, 119, 5770-5805.
  • polymer classes that have already been used in the electrospinning process.
  • thermoplastics are used for electrospinning as a melt or dissolved in a suitable solvent as a solution.
  • Electrospun fleeces are used for filtration, for example in respiratory masks for occupational and infection protection, as well as in room air purification devices, in which the contaminated air is sucked into a container through an air inlet opening by means of a fan and passed through a series of filters.
  • Fiber fleeces with fiber diameters from a few micrometers to a few Nanometers are particularly suitable for use as filter media because they are characterized by a low pressure drop and a high filtration efficiency of the filter medium.
  • the filter effect is based, among other things, on the large specific surface area of the nanofibers, and the lower pressure drop and thus breathing resistance is due to the high porosity of the corresponding fiber fleece.
  • the use of electrets is also known to increase the filtration efficiency of air and breathing filters.
  • Autoclavable or sterilizable filter media require the filter medium to be sufficiently stable against temperature or ionizing radiation.
  • thermoplastics such as polyester or polypropylene cannot be used for this purpose, but special, high-melting thermoplastics such as polyimide (PI) or polyetherimide (PEI) are required.
  • PI polyimide
  • PEI polyetherimide
  • silicone elastomers which are temperature- or UV-crosslinkable systems.
  • the base components are typically soluble in most aprotic solvents and, due to their mostly thinning properties, pumpable and thus easy to process.
  • silicone elastomers are characterized by high mechanical flexibility and stability against temperature and radiation effects.
  • silicones which are found at the negative end of the triboelectric series, are characterized by a particularly high electron affinity on the material surface and can therefore function well as electrets.
  • the electrospinning of silicones is also known in the art and is typically carried out from an organic solvent.
  • a crosslinkable silicone composition made of polymethylhydrogensiloxane, (DVi) 4 and JUPtCle
  • PVP polyvinylpyrrolidone
  • silicones are suitable for coaxial electrospinning processes, where they are electrospun together with immiscible, usually hydrophilic polymers without prior mixing, so that core-shell fibers are obtained.
  • the outer shell polymer serves as a template for the formation of fibers.
  • non-flammable organic solvents such as chloroform or solvents with a high flash point such as DMF can also be added to the spinning solutions, but these must be viewed particularly critically from the point of view of health and environmental protection.
  • the water-insoluble polymer particles are stabilized using an emulsifier.
  • a water-soluble polymer that acts as a thickener known as a template polymer. This helps to promote fiber formation from the colloidal polymer dispersion (electrospinning) compared to spraying (electrospraying).
  • condensation crosslinking of silicone elastomers is in particular the higher crosslinking speed compared to addition crosslinking or Radical cross-linking results in a lower reaction rate and an incomplete reaction, so that a residual silanol content in the cured material is unavoidable.
  • polar OH groups can have a negative effect on the electret properties of the spun material.
  • the condensation cross-linking of silicones is accompanied by shrinkage and the by-products produced in stoichiometric amounts (such as water) can lead to undesirable porosity of the fibers.
  • the fiber diameters disclosed in the example are 1 to 5 pm, so that no nanofibers are obtained with this system. Since no washing step is disclosed, it can be assumed that these are not pure silicone fibers.
  • the compaction of the nonwoven structure can be avoided or at least reduced by replacing the water with an organic solvent with a lower surface tension
  • the use of organic solvents can lead to swelling of the silicone nanofibers and the use of organic solvents must also be critically evaluated with regard to occupational safety and environmental protection.
  • the task is therefore to provide silicone dispersions in order to use them in an improved electrospinning process to produce silicone nanofibers so that the above-mentioned disadvantages of the state of the art no longer occur.
  • the present invention therefore relates to a
  • (Z) at least one silicone elastomer composition which is selected from addition-crosslinking or radically crosslinking silicone elastomer compositions, wherein the sum of the amounts of (Y) and (Z) used in the electrospinning dispersion is 4 to 50 wt. %.
  • the electrospinning dispersion according to the invention can be either a silicone emulsion or a suspension.
  • Processes for their preparation have long been known to the person skilled in the art from the prior art. Production is usually carried out by simply stirring all the components and, if necessary, subsequent homogenization with jet dispersers, rotor-stator homogenizers, colloid mills or high-pressure homogenizers.
  • the known methods are also suitable for producing the electrospinning dispersion according to the invention.
  • the sum of the amounts of (Y) and (Z) used in the electrospinning dispersion is preferably 8 to 35 wt.%.
  • the ratio of (Z) to (Y) is usually between 0.25 and 10.0, preferably between 0.5 and 8.0.
  • (Y) contains at least one hydrophilic polymer.
  • the ratio of (Z) to (Y) is between 0.25 and 4.0, preferably 0.5 to 3.0, particularly preferably 0.8 to 2.5.
  • the electrospinning dispersion according to the invention usually contains 50 to 96 wt.%, preferably 60 to 92 wt.% water (X).
  • the components (Z) and (Y) and any other optional components (W) are used in such amounts that, together with the water (X), they always add up to 100% by weight.
  • Water is used as component (X). To avoid possible problems caused by salt deposits during the subsequent spinning process, it is preferable to use fully demineralized water.
  • component (Y) at least one emulsifier and/or at least one hydrophilic polymer is used.
  • component (Y) can therefore be:
  • the electrospinning dispersion according to the invention preferably contains 0.4 to 40 wt. %, particularly preferably 4 to 20 wt. % (Y). Hydrophilic polymer (Y)
  • the hydrophilic polymer can be a homopolymer, copolymer, block polymer, graft copolymer, star polymer, highly branched polymer, dendrimer or a mixture of two or more of the aforementioned polymer types.
  • Suitable water-soluble polymers (Y) are, for example, polyvinyl alcohol, polyvinyl formamide, polyvinylamine, polycarboxylic acid (polyacrylic acid, polymethacrylic acid), polyacrylamide, polyitaconic acid, poly(2-hydroxyethyl acrylate), poly(N-isopropylacrylamide), polysulfonic acid (e.g.
  • copolymers, block polymers, graft copolymers, Star polymers, highly branched polymers or dendrimers are possible, which are composed of a combination of two or more of the above-mentioned polymer-forming monomer units.
  • the water-soluble polymer is selected from the group containing polyvinyl alcohol, polyethylene oxides, poly-N-vinylpyrrolidone, polyvinyl formamide. Polyvinyl alcohol is particularly preferred.
  • Polyvinyl alcohols used as component (Y) can be partially saponified or fully saponified polyvinyl alcohols, for example with a degree of hydrolysis of 80 to 100 mol%, in particular partially saponified polyvinyl alcohols with a degree of hydrolysis of 80 to 95 mol%, preferably 85 to 92 mol%.
  • the polyvinyl alcohols have a Höppler viscosity in 4% aqueous solution of preferably 1 to 130 mPas (Höppler method at 20 °C, DIN 53015).
  • Examples of these are partially saponified copolymers of vinyl acetate with hydrophobic comonomers such as isopropenyl acetate, vinyl pivalate, vinyl ethyl hexanoate, vinyl esters of saturated alpha-branched monocarboxylic acids with 5 or 9 to 11 C atoms, dialkyl maleates and dialkyl fumarates such as diisopropyl maleate and diisopropyl fumarate, vinyl chloride, vinyl alkyl ethers such as vinyl butyl ether, olefins such as ethene and decene.
  • the proportion of hydrophobic units is preferably 0.1 to 10% by weight, based on the total weight of the partially saponified polyvinyl alcohol. Mixtures of the above-mentioned polyvinyl alcohols can also be used.
  • polyvinyl alcohols with a degree of hydrolysis of 85 to 94 mol-% and a Höppler viscosity, in 4% aqueous solution, of 3 to 48 mPas (Höppler method at 20 °C, DIN 53015).
  • emulsifier refers to surface-active substances (also known as surfactants) that are typically used as dispersing aids, regardless of whether the electrospinning dispersion in the present case is actually an emulsion or a suspension.
  • emulsifier (Y) for preparing the electrospinning dispersions according to the invention, both individually and as mixtures of at least two emulsifiers with which aqueous dispersions, in particular aqueous emulsions of organopolysiloxanes.
  • anionic emulsifiers are:
  • Alkyl sulfates especially those with a chain length of 8 to 18 C atoms, alkyl and alkaryl ether sulfates with 8 to 18 C atoms in the hydrophobic residue and 1 to 40 ethylene oxide (EO) or propylene oxide (PO) units.
  • EO ethylene oxide
  • PO propylene oxide
  • Sulfonates particularly alkylsulfonates with 8 to 18 C atoms, alkylarylsulfonates with 8 to 18 C atoms, taurides, esters and half-esters of sulfosuccinic acid with monohydric alcohols or alkylphenols with 4 to 15 C atoms; these alcohols or alkylphenols may optionally also be ethoxylated with 1 to 40 EO units.
  • Partial phosphoric acid esters and their alkali and ammonium salts particularly alkyl and alkaryl phosphates with 8 to 20 C atoms in the organic radical, alkyl ether or alkaryl ether phosphates with 8 to 20 C atoms in the alkyl or alkaryl radical and 1 to 40 EO units.
  • non-ionic emulsifiers Y
  • Y ⁇ ionic emulsifiers
  • Alkyl polyglycol ethers preferably those having 3 to 40 EO units and alkyl radicals of 8 to 20 C atoms.
  • Alkylaryl polyglycol ethers preferably those having 5 to 40 EO units and 8 to 20 C atoms in the alkyl and aryl radicals.
  • Ethylene oxide/propylene oxide (EO/PO) block copolymers preferably those with 8 to 40 EO or PO units.
  • Natural substances and their derivatives such as lecithin, lanolin, saponins, cellulose, cellulose alkyl ethers and carboxyalkyl celluloses, whose alkyl groups each have up to 4 carbon atoms.
  • Linear organo(poly)siloxanes containing polar groups in particular the elements O, N, C, S, P, Si, in particular those with alkoxy groups with up to 24 C atoms and/or up to 40 EO and/or PO groups.
  • cationic emulsifiers are:
  • Alkylpyridinium, alkylimidazolinium and alkyloxazolinium salts in particular those whose alkyl chain has up to 18 C atoms, especially the halides, sulfates, phosphates and acetates.
  • amphoteric emulsifiers Y
  • Long-chain substituted amino acids such as N-alkyl-di-(aminoethyl-)glycine or N-alkyl-2-aminopropionic acid salts.
  • Betaines such as N-(3-acylamidopropyl)-N,N-dimethylammonium salts with a C1-C4-Acyl radical and alkylimidazolium betaines or quaternized alkyl or substituted alkyl derivatives of N,N-dimethylglycine.
  • Preferred emulsifiers (Y) for the preparation of electrospinning dispersions according to the invention are selected from the group of nonionic emulsifiers, in particular from the alkyl polyglycol ethers listed above under 6.
  • Component (Y) can consist of one of the abovementioned emulsifiers (Y) or of a mixture of two or more of the abovementioned emulsifiers (Y); it can be used in pure form or as solutions of one or more emulsifiers (Y) in water or organic solvents.
  • the silicone elastomer composition used according to the invention is selected from addition-crosslinking or radically crosslinking silicone elastomer compositions.
  • the electrospinning dispersion according to the invention preferably contains 0.8 to 45 wt. %, particularly preferably 5.0 to 23 wt. % (Z).
  • the compounds (A) and (B) or (C) used in the addition-crosslinking silicone elastomer compositions (Z) according to the invention are known to be selected so that crosslinking is possible.
  • compound (A) has at least two aliphatically unsaturated radicals and (B) at least three Si-bonded hydrogen atoms
  • compound (A) has at least three aliphatically unsaturated radicals and siloxane (B) has at least two Si-bonded hydrogen atoms
  • siloxane (C) is used, which has aliphatically unsaturated radicals and Si-bonded hydrogen atoms in the abovementioned ratios.
  • Mixtures of (A) and (B) and (C) with the above-mentioned ratios of aliphatically unsaturated radicals and Si-bonded hydrogen atoms are also possible.
  • the silicone compositions according to the invention preferably contain at least one aliphatically unsaturated organosilicon compound as component (A), whereby all aliphatically unsaturated organosilicon compounds previously used in addition-crosslinking compositions can be used, such as, for example, silicone block copolymers with Urea segments, silicone block copolymers with amide segments and/or imide segments and/or ester-amide segments and/or polystyrene segments and/or silarylene segments and/or carborane segments and silicone graft copolymers with ether groups.
  • silicone block copolymers with Urea segments silicone block copolymers with amide segments and/or imide segments and/or ester-amide segments and/or polystyrene segments and/or silarylene segments and/or carborane segments and silicone graft copolymers with ether groups.
  • organosilicon compounds (A) which have Si-C-bonded radicals with aliphatic carbon-carbon multiple bonds, preferably linear or branched organopolysiloxanes comprising units of the general formula (I)
  • R 4 independently of one another, identical or different, is an organic or inorganic radical free from aliphatic carbon-carbon multiple bonds
  • R 5 independently of one another, identically or differently, denotes a monovalent, substituted or unsubstituted, Si-C-bonded hydrocarbon radical having at least one aliphatic carbon-carbon multiple bond, a is 0, 1, 2 or 3, and b is 0, 1 or 2, with the proviso that the sum a + b is less than or equal to 3 and at least 2 R 5 radicals are present per molecule.
  • the residue R 4 can be monovalent or polyvalent, whereby the polyvalent residues , such as bivalent , trivalent and tetravalent residues , then several , such as about two, three or four siloxy units of the formula (I) are connected to each other.
  • R 4 are the monovalent radicals -F, -Cl, - Br, -OR 6 , -CN, -SCN, -NCO and Si-C-bonded, substituted or unsubstituted hydrocarbon radicals which can be interrupted by oxygen atoms or the group -C(O)-, as well as divalent radicals which are Si-bonded on both sides according to formula (I).
  • radical R 4 is a Si-C-bonded, substituted hydrocarbon radical
  • preferred substituents are halogen atoms, phosphorus-containing radicals, cyano radicals, -OR 6 , -NR 6 -, - NR 6 2, -NR 6 -C (0) -NR 6 2, - C(0)— NR 6 2, -C(O)R 6 , -C(O)OR 6 , -SO 2 -Ph and - CeFs.
  • R 6 independently, identically or differently represents a hydrogen atom or a monovalent hydrocarbon radical having 1 to 20 carbon atoms and Ph represents the phenyl radical.
  • radicals R 4 are alkyl radicals, such as the methyl, ethyl, n-propyl, iso-propyl, n-butyl, iso-butyl, tert-butyl, n-pentyl, iso-pentyl, neo-pentyl, tert-pentyl radical, hexyl radicals, such as the n-hexyl radical, heptyl radicals, such as the n-heptyl radical, octyl radicals, such as the n-octyl radical and iso-octyl radicals, such as the 2,2,4-trimethylpentyl radical, nonyl radicals, such as the n-nonyl radical, decyl radicals, such as the n-decyl radical, dodecyl radicals, such as the n-dodecyl radical, and octadecyl radical
  • substituted radicals R 4 are haloalkyl radicals, such as the 3, 3, 3-trifluoro-n-propyl radical, the 2 , 2 , 2 , 2 ' , 2 ' , 2 '- Hexafluoroisopropyl radical, the heptafluoroisopropyl radical, haloaryl radicals such as the o-, m- and p-chlorophenyl radical, - (CH2)-
  • R 4 divalent radicals which are Si-bonded on both sides according to formula (I) are those which are derived from the monovalent examples given above for radical R 4 in that an additional bond occurs through substitution of a hydrogen atom.
  • examples of such radicals are - (CH 2 )-, -CH(CH 3 )-, -C(CH 3 ) 2 -, -CH (CH 3 ) -CH 2 -, -C 6 H 4 -, -CH (Ph) -CH 2 -, -C(CF 3 ) 2 -, - (CH 2 ) OC 6 H 4 - (CH 2 ) O-, - (CH 2 ) OC 6 H 4 -C 6 H 4 - (CH 2 ) O-, - (CH 2 0)p, (CH 2 CH 2 0) O, - (CH 2 ) O-0X-C6H 4 -S02-C 6 H 4 -0X- (CH2) O-, where x is 0 or
  • the radical R 4 is preferably a monovalent, Si-C-bonded, optionally substituted hydrocarbon radical having 1 to 18 carbon atoms and free from aliphatic carbon-carbon multiple bonds, particularly preferably a monovalent, Si-C-bonded hydrocarbon radical having 1 to 6 carbon atoms and free from aliphatic carbon-carbon multiple bonds, in particular the methyl or phenyl radical.
  • the radical R 5 in formula (I) can be any group that is accessible to an addition reaction (hydrosilylation) with a SiH-functional compound. If the radical R 5 is a Si-C-bonded, substituted hydrocarbon radical, halogen atoms, cyano radicals and -OR 6 are preferred as substituents, where R 6 has the meaning given above.
  • the radical R 5 preferably comprises alkenyl and alkynyl groups having 2 to 16 carbon atoms, such as vinyl, allyl, methallyl, 1-propenyl, 5-hexenyl, ethynyl, butadienyl, hexadienyl, cyclopentenyl, cyclopentadienyl, cyclohexenyl, vinylcyclohexylethyl, divinylcyclohexylethyl, norbornenyl, vinylphenyl and styryl radicals, with vinyl, allyl and hexenyl radicals being particularly preferably used.
  • alkenyl and alkynyl groups having 2 to 16 carbon atoms such as vinyl, allyl, methallyl, 1-propenyl, 5-hexenyl, ethynyl, butadienyl, hexadienyl, cyclopentenyl, cyclopentadienyl
  • component (A) can vary within wide limits, for example between 10 2 and 10 6 g/mol .
  • component (A) can be a relatively low molecular weight alkenyl-functional oligosiloxane, such as 1,2-divinyltetramethyldisiloxane, but also a high-polymer polydimethylsiloxane having chain-positioned or terminal Si-bonded vinyl groups, e.g. with a molecular weight of 10 5 g/mol (number average determined by NMR).
  • the structure of the molecules forming component (A) is also not fixed; in particular, the structure of a higher molecular weight, i.e.
  • oligomeric or polymeric siloxane can be linear, cyclic, branched or even resinous, network-like.
  • Linear and cyclic polysiloxanes are preferably composed of units of the formula R 4 3SiOi/2 , R 5 R 4 2SiOi/2 , R 5 R 4 SiOi/2 and R 4 2SiO2/2 , where R 4 and R 5 have the meaning given above.
  • Branched and network-like polysiloxanes additionally contain trifunctional and/or tetrafunctional units, with those of the formulae R 4 SiO3/2 , R 5 SiO3/2 and S1O4/2 being preferred. Mixtures can of course also be used.
  • different siloxanes that satisfy the criteria of component (A) can be used.
  • component (A) is the use of vinyl-functional, essentially linear polydiorganosiloxanes having a viscosity of 0.1 to 800,000 mPa-s, particularly preferably 0.1 to 200,000 mPa-s, in each case at 25°C, measured according to DIN EN ISO 3219: 1994 and DIN 53019 by means of a calibrated rheometer with a cone-plate system, cone CP50-2 with an opening angle of 2° and a shear rate of 0.1 s ⁇ 4 .
  • organosilicon compounds (B) All hydrogen-functional organosilicon compounds which have previously been used in addition-crosslinkable compositions can be used as organosilicon compounds (B).
  • organopolysiloxanes (B) containing Si-bonded hydrogen atoms preferably linear, cyclic or branched organopolysiloxanes consisting of units of the general formula (III)
  • R 4 has the meaning given above, c is 0,1, 2 or 3 and d is 0, 1 or 2, with the proviso that the sum of c + d is less than or equal to 3 and at least two Si-bonded hydrogen atoms are present per molecule.
  • the organopolysiloxane (B) used according to the invention contains Si-bonded hydrogen in the range from 0.04 to 1.7 percent by weight, based on the total weight of the organopolysiloxane (B).
  • the molecular weight of the component (B) can also vary within wide limits, for example between 102 and 106 g/mol.
  • the component (B) can be a relatively low molecular weight SiH-functional oligosiloxane, such as tetramethyldisiloxane, but also a high-polymer polydimethylsiloxane having chain- or terminal SiH groups or a silicone resin having SiH groups.
  • the structure of the molecules forming component (B) is also not fixed; in particular, the structure of a higher molecular weight, i.e. oligomeric or polymeric SiH-containing siloxane can be linear, cyclic, branched or also resinous, network-like.
  • Linear and cyclic polysiloxanes (B) are preferably composed of units of the formula R 4 3SiOi/2 , HR 4 2SiOi/2 , HR 4 SiO2/2 and R 4 2SiO2/2 , where R 4 has the meaning given above.
  • Branched and network-like polysiloxanes additionally contain trifunctional and/or tetrafunctional units, with those of the formulae R 4 SiO3/2 , HS1O3/2 and S1O4/2 being preferred, where R 4 has the meaning given above.
  • component (B) can optionally also contain aliphatically unsaturated groups in addition to the obligatory SiH groups.
  • Particularly preferred is the use of low molecular weight SiH-functional compounds such as tetrakis(dimethylsiloxy)silane and tetramethylcyclotetrasiloxane, as well as higher molecular weight, SiH-containing siloxanes such as poly(hydrogenmethyl)siloxane and poly(dimethylhydrogenmethyl)siloxane with a viscosity at 25°C of 10 to 20,000 mPa-s, measured according to DIN EN ISO 3219: 1994 and DIN 53019 using a calibrated rheometer with a cone-plate system, cone CP50-2 with an opening angle of 2° and a shear rate of 0.1 s -1 , or analogous SiH-containing compounds in which some of the methyl
  • Component (B) is preferably present in the crosslinkable silicone compositions according to the invention in an amount such that the molar ratio of SiH groups to aliphatically unsaturated groups from (A) is from 0.1 to 20, particularly preferably between 0.3 and 2.0.
  • the components (A) and (B) used according to the invention are commercially available products or can be produced by conventional processes.
  • the silicone compositions according to the invention can contain organopolysiloxanes (C) which simultaneously have aliphatic carbon-carbon multiple bonds and Si-bonded hydrogen atoms.
  • the silicone compositions according to the invention can also contain all three components (A), (B) and (C).
  • siloxanes (C) are preferably those consisting of units of the general formulas (IV), (V) and (VI) R 4 fSiO 4 /2 (IV)
  • R 4 and R 5 have the meaning given above, f is 0, 1, 2 or 3, g is 0, 1 or 2 and h is 0, 1 or 2, with the proviso that at least two R 5 radicals and at least two Si-bonded hydrogen atoms are present per molecule.
  • organopolysiloxanes (C) are those consisting of S1O4/2, R 4 3SiOi/2-, R 4 2R 5 SiOi/2- and R 4 2HSiOi/2- units, so-called MQ resins, whereby these resins can additionally contain R 4 SiO3/2- and R 4 2SiO units, as well as linear organopolysiloxanes essentially consisting of R 4 2R 5 SiOi/2-, R 4 2SiO- and R 4 HSiO units with R 4 and R 5 equal to the meaning given above.
  • the organopolysiloxanes (C) preferably have an average viscosity of 0.01 to 800,000 Pa-s, particularly preferably 0.1 to 200,000 Pa-s, each at 25°C, measured according to DIN EN ISO 3219: 1994 and DIN 53019 by means of a calibrated rheometer with a cone-plate system, cone CP50-2 with an opening angle of 2° and a shear rate of 0.1 s ⁇ 4 .
  • Organopolysiloxanes (C) are commercially available or can be prepared using conventional methods.
  • the addition-crosslinking silicone elastomer composition (Z) according to the invention usually contains 30-95 wt.%, preferably 30-80 wt.% and particularly preferably 35-70 wt.% (A), based on the total mass of the addition-crosslinking silicone elastomer composition (Z).
  • the addition-crosslinking silicone elastomer composition (Z) according to the invention usually contains 0.1-60 wt.%, preferably 0.5-50 wt.% and particularly preferably 1-40 wt.% (B), based on the total mass of the addition-crosslinking silicone elastomer composition.
  • addition-crosslinking silicone elastomer composition (Z) according to the invention contains component (C), usually 30-95% by weight, preferably 30-80% by weight, particularly preferably 40-70% by weight of (C) are contained in the formulation, based on the total mass of the addition-crosslinking silicone elastomer composition (Z).
  • Component (D) can be a platinum group metal, for example platinum, rhodium, ruthenium, palladium, osmium or iridium, an organometallic compound or a combination thereof.
  • component (D) are compounds such as hexachloroplatinic (IV) acid, platinum dichloride, platinum acetylacetonate and complexes of said compounds encapsulated in a matrix or a core-shell-like structure.
  • the low molecular weight platinum complexes of the organopolysiloxanes include 1,3-diethenyl-1,1,3,3-tetramethyldisiloxane complexes with platinum.
  • platinum phosphite complexes platinum phosphine complexes or alkylplatinum complexes. These Compounds can be encapsulated in a resin matrix.
  • Suitable hydrosilylation catalysts (D) are also those which can be activated by electromagnetic radiation (UV, UV-VIS, IR). Such catalysts have also been known from the state of the art for a long time. Examples of these are (r
  • the concentration of component (D) in the addition-curing silicone elastomer composition (Z) is sufficient to catalyze the hydrosilylation reaction of components (A) and (B) when exposed to generate the heat required in the process described herein.
  • the amount of component (D) may be between 0.1 and 1000 parts per million (ppm), 0.5 and 100 ppm, or 1 and 50 ppm of the platinum group metal, depending on the total weight of the components.
  • the cure rate may be low if the platinum group metal content is less than 1 ppm. Use of more than 100 ppm of the platinum group metal is uneconomical or may reduce the stability of the adhesive formulation.
  • Fillers such as pyrogenic or precipitated silica, or resinous, i.e. three-dimensionally cross-linked polyorganosiloxanes, which are different from (A), (B) and (C), can be used as component (E).
  • Reinforcing fillers such as pyrogenic or precipitated silica with BET surface areas between 50 m 2 /g and 400 m 2 /g are preferred, with pyrogenic and precipitated silica with BET surface areas of between 100 m 2 /g and 300 m 2 /g being particularly preferred.
  • the silica fillers mentioned can be hydrophilic in nature or can be hydrophobized using known processes.
  • surface-treated silicas (E) are used.
  • the surface treatment is achieved by the methods known in the art for hydrophobizing finely divided fillers.
  • Preferred fillers (E) have a carbon content of at least 0.01 to a maximum of 20% by weight, preferably between 0.1 and 10% by weight, particularly preferably between 0.5 and 5% by weight, as a result of a surface treatment.
  • Particularly preferred are crosslinkable addition-crosslinking silicone elastomer compositions (Z) which are characterized in that the filler (E) is a surface-treated silica containing 0.01 to 2% by weight of Si-bonded, aliphatically unsaturated groups. These are, for example, Si-bonded vinyl groups.
  • the three-dimensionally cross-linked polyorganosiloxanes which are also preferred as component (E), and which differ from (A), (B) and (C), are so-called organosiloxane resins which are composed of units of the general formulas (VII), (VIII), (IX) and (X)
  • R is selected from R , R , OH and OR 2 , and with the proviso that at least 20 mol% of the units are selected from units of the general formulas (IX) and (X) , and at most 2 wt.% of the radicals R are OH.
  • R 1 is an identical or independently different monovalent organofunctional hydrocarbon radical, an unsaturated hydrocarbon radical or a hydrogen radical, where the radical R 1 is bonded to the silicon atom via a carbon atom or the hydrogen radical is bonded directly to the silicon atom.
  • R 1 is preferably an alkenyl group or the hydrogen radical.
  • the vinyl group is particularly preferred as R 1 .
  • R are identical or independently different monovalent hydrocarbon radicals (alkyl, aryl, aralkyl). 2
  • unsubstituted radicals R are alkyl radicals, such as the methyl, ethyl, n-propyl, isopropyl, n-butyl, isobutyl, tert.-butyl, n-pentyl, isopentyl, neopentyl, tert.-pentyl radical, hexyl radicals, such as the n-hexyl radical, heptyl radicals, such as the n-heptyl radical, octyl radicals, such as the n-octyl radical and isooctyl radicals, such as the 2,2,4-trimethylpentyl radical, nonyl radicals, such as the n-nonyl radical, decyl radicals, such as the n-decyl radical; Alkenyl radicals, such as vinyl, allyl, n-5-hexenyl, 4-vinylcyclohexy
  • substituted hydrocarbon radicals as R radicals are halogenated hydrocarbons such as the chloromethyl, 3-chloropropyl, 3-bromopropyl, 3,3,3-trifluoropropyl and 5,5,5,4,4,3,3-heptafluoropentyl radical as well as the chlorophenyl, dichlorophenyl and trifluorotolyl radicals.
  • R preferably has 1 to 6 carbon atoms. Methyl and phenyl are particularly preferred.
  • the preferred radicals R are methyl, ethyl, phenyl and vinyl.
  • organosiloxane resins (E) preferably contain at least 30 mol%, in particular at least 40 mol% and preferably at most 80 mol%, in particular at most 70 mol% of units of the general formulas (IX) and (X).
  • organosiloxane resins (E) are preferably MQ silicone resins (MQ) which contain at least 80 mol% units, preferably at least 95 mol%, in particular at least 97 mol% units of the general formulas (VII) and (X).
  • the average ratio of the units of the general formulas (VII) to (X) is preferably at least 0.25, in particular at least 0.5 and preferably 2, particularly preferably at most 1.5.
  • radicals R are OH.
  • At least 0.01 mol%, particularly preferably at least 0.05 mol%, and preferably at most 8 mol%, in particular at most 5 mol% of the radicals R denote an R 1 .
  • the average molecular weight Mn of the organosiloxane resins (E) is preferably at least 200 g/mol, in particular at least 1000 g/mol and preferably at most 100,000 g/mol, in particular at most 20,000 g/mol.
  • the component (E) is preferably used as a single or likewise preferably as a mixture of several finely divided fillers.
  • the addition-crosslinking silicone elastomer composition (Z) according to the invention preferably contains 0 to 45 wt.% (E), particularly preferably 0-35 wt.% (E).
  • addition-crosslinking silicone compositions according to the invention can optionally contain all other additives which are known to the person skilled in the art for addition-crosslinkable compositions.
  • additives can be, for example, rheological additives, inhibitors, light stabilizers, flame retardants, dispersants, heat stabilizers, etc.
  • the amounts used for each individual component of the silicone elastomer composition (Z) are selected such that they always add up to 100% by weight.
  • Peroxide-crosslinking silicone elastomer compositions have long been known to the person skilled in the art from the prior art.
  • Peroxide-crosslinking silicone elastomer compositions are preferred: in the simplest case, these contain at least one organopolysiloxane with at least 2 crosslinkable groups per molecule, such as methyl or vinyl groups, and at least one suitable organic peroxide as a catalyst.
  • suitable organic peroxides are acyl peroxides, such as dibenzoyl peroxide, bis-(4-chlorobenzoyl) peroxide, bis-(2,4-dichlorobenzoyl) peroxide and bis-(4-methylbenzoyl) peroxide;
  • Alkyl peroxides and aryl peroxides such as di-tert-butyl peroxide, 2,5-bis-(tert-butylperoxy)-2,5-dimethylhexane, dicumyl peroxide and 1,3-bis-(tert-butylperoxy-isopropyl)-benzene; perketals such as l,l-bis-(tert-butylperoxy)-3,3,5-trimethyl 1 cyclohexane; peresters such as diacetyl peroxydicarbonate, tert-butyl perbenzoate, tert-butylperoxy-isopropyl carbonate, tert-butylperoxy-isononanoate, dicyclohexyl peroxydicarbonate and 2,5-dimethylhexane-2,5-diperbenzoate.
  • One type of organic peroxide or a mixture of at least two different types of organic peroxides can be used
  • the radically crosslinking composition according to the invention contains Silicone elastomer composition (Z) at least one aliphatically unsaturated organosilicon compound (A) and a photoinitiator.
  • the radically crosslinking silicone elastomer composition (Z) additionally contains at least one mercaptoalkyl-functional polydiorganosiloxane (M) of the general formula (XI):
  • R 12 is selected from mercaptomethyl, mercaptoethyl, mercaptopropyl,
  • R 10 , R 11 , R 8 , R 9 and R 13 are independently selected from C1-C2 O-hydrocarbon radicals (alkyl+aryl), and
  • At least one mixed functionalized mercaptoalkyl-functional polydiorganosiloxane (N) can also be used with the general formula (XI I)
  • R 8 , R 9 , R 10 , R 11 , R 13 , y and z have the meaning given above, with the proviso that if R 14 is a sulphur-containing group, R 15 must be a sulphur-free group or . if R 14 is a sulfur-free group, R 15 must be a sulfur-containing group .
  • the radically crosslinking silicone elastomer composition (Z) may also contain the above-mentioned components (E).
  • the electrospinning dispersions according to the invention can optionally contain further ingredients.
  • such components are salts, pH regulators, foam inhibitors, thickeners and/or protective colloids, preservatives, disinfectants, wetting agents, corrosion inhibitors, dyes, fragrances or mixtures thereof.
  • salts are added specifically, they serve as conductive salts in order to ensure or improve the electrospinnability of the electrospinning dispersion.
  • Such conductive salts are suitable for the defined adjustment of the electrical conductivity and have long been known in the electrochemical industry.
  • these conductive salts can be inorganic, organic salts or mixtures thereof.
  • Thermally labile salts such as pyridinium formate and ammonium formate are preferably used as conductive salts.
  • components (W) are used, they are preferably first added to one of the components (X) or (Y), particularly preferably to the water (X).
  • Another object of the present invention is a process for producing nonwovens in which in a first step, the electrospinning dispersion according to the invention is prepared by mixing all of the components according to the invention, in a second step, a nonwoven fabric made of fibers is produced from this electrospinning dispersion by means of electrospinning, wherein the crosslinking of the silicone composition (Z) is initiated or not initiated thermally or by means of electromagnetic radiation, in a third step, the crosslinking of the silicone composition (Z) is completely cured thermally or by means of electromagnetic radiation, in a fourth step, (Y) is washed out of the nonwoven fabric at least once with at least one protic polar solvent (i), in a fifth step, the washed nonwoven fabric is dried by means of sublimation.
  • the fibres of the fleece produced in this way preferably have a diameter of less than 1 pm.
  • the protic polar solvent (i) used for this purpose can also be a mixture (i) of at least two (i) which contains 30 to 100% by weight of water.
  • (i) contains 50 to 100% by weight, particularly preferably 85% to 100% by weight of water.
  • Other components of (i) can be alcohols such as methanol, ethanol and isopropanol or surface-active substances such as surfactants or emulsifiers.
  • the fourth step is performed using ultrasound treatment.
  • freeze-drying i.e. drying via sublimation
  • drying via sublimation is an essential step of the invention, in which there is no compaction of the fleece structure and therefore no loss of porosity.
  • the washed fleece which is still wetted with (i), is frozen at temperatures below the freezing point of (i). Then (i) is dried at a reduced pressure of 0.001 to 800 mbar by means of sublimation with possible further cooling of the fleece below the freezing point of
  • the sublimation is carried out at constant reduced pressure with increasing temperature control.
  • the fleece spread out flat is covered with water so that the fleece is just completely covered, frozen and then dried at constant reduced pressure with increasing temperature control.
  • the negative pressure is preferably in the range of 0.01 to 500 mbar.
  • the increasing temperature control begins at a temperature below the freezing point of water, particularly preferably in a range of -10 °C to -50 °C.
  • the end point of the increasing temperature control is above the freezing point of water, preferably in a range of 0 °C to 50 °C and particularly preferably in a range of 5 to 25 °C.
  • the temperature increase takes place in the form of a Temperature staircase, i.e. stepwise.
  • the increase is in steps of 5 to 10 °C.
  • the holding time of a temperature step is in the range of 0.1 to 24 h, preferably in the range of 0.5 to 10 h.
  • the possible start of crosslinking in the second step and the complete curing in the third step of the silicone composition (Z) is preferably carried out thermally, preferably at 20°C to 250°C, preferably at least 50°C, in particular at least 100°C, preferably at 120-210°C.
  • the thermal curing is carried out, for example, by means of a heatable collector, by means of infrared radiation with a wavelength of 780 nm to 1 mm or by means of an oven.
  • crosslinking is carried out by irradiation, this is carried out with light of wavelength 230-450 nm, preferably for at least 1 second, particularly preferably at least 5 seconds and preferably at most 500 seconds, particularly preferably at most 240 seconds.
  • the irradiation with light preferably lasts for at least 1 second, particularly preferably at least 5 seconds and preferably at most 500 seconds, particularly preferably at most 240 seconds.
  • Crosslinking with photoinitiators can be carried out under protective gas such as N2 or Ar or under air.
  • the irradiated fibers are optionally thermally post-treated and then preferably heated for a maximum of 1 hour, particularly preferably a maximum of 10 minutes, in particular a maximum of 5 minutes, in order to cure them.
  • Crosslinking is particularly preferably carried out with light of wavelength 230-450 nm, in particular at 254 to 450 nm.
  • the reaction underlying the crosslinking of the silicone composition (Z) can take place at least partially during the electrospinning process. This can be brought about in particular by heating the ambient air or irradiating it with IR or UV radiation during electrospinning.
  • the silicone composition can be crosslinked at a later time, so that the third step is carried out separately from the second step and after it.
  • a further subject matter of the present invention are the cross-linked nonwovens according to the invention produced by the process according to the invention.
  • a further subject matter of the present invention is the use of the cross-linked nonwovens according to the invention as a coating of three-dimensional structures, in wound plasters, in packaging materials, and also in filters and membranes.
  • the nonwovens according to the invention are suitable as a coating for three-dimensional structures in order to change their surface properties with regard to, for example, sound or thermal insulation, shock absorption.
  • the breathability that can be achieved with the coating can represent a desired additional property.
  • Housings, building materials or textiles are preferably coated or laminated with the nonwovens according to the invention.
  • the nonwovens according to the invention can also preferably be used in wound plasters.
  • nonwovens according to the invention can also be used as bacteriophobic and/or antimicrobial coating.
  • nonwovens according to the invention are also preferred, in particular in the packaging of foodstuffs.
  • the nonwovens according to the invention are also suitable as a coating for containers for storing liquids, so that the containers can be completely emptied.
  • the nonwovens according to the invention can also be used particularly preferably in clothing items, such as jackets, gloves, hats or shoes, or as roofing membranes.
  • the nonwovens according to the invention are water-repellent and breathable.
  • the nonwovens according to the invention can particularly preferably also be used as filter media, e.g. for air filters or for separating particles from gas or liquid streams.
  • the nonwovens according to the invention can in particular also be used as filter media in respiratory masks, e.g. in FFP3 and FFP2 masks.
  • the nonwovens according to the invention can also be used as membranes for separating mixtures, such as reverse osmosis, gas separation, pervaporation, nanofiltration, ultrafiltration or microfiltration. Solid-solid, gaseous-gaseous, solid-gaseous or liquid-gaseous, in particular liquid-liquid, solid-gaseous and liquid-solid mixtures can be separated. If the nonwovens according to the invention are used as membranes, they can be installed in the common modules, such as hollow fiber modules, spiral wound modules, plate modules, cross-flow modules or dead-end modules. The nonwovens according to the invention can also be used as a carrier or support layer for other membranes.
  • the silicone composition was mixed in a laboratory mixer from VMA-Getzmann GmbH with a toothed dissolver disk (diameter 40 mm).
  • Hydrophobic silica HDK® H30 fumed silica with dimethylsiloxy groups, BET surface area: 250 m2/g, tamped density: 40 g/ml (available from WACKER Chemie AG).
  • component ( Z )
  • the two-component, thermally addition-curing silicone elastomer LUMIS IL® LR 7601/60 consisting of an A and a B component available from Wacker Chemie AG was used as silicone composition 3A and 3B.
  • the particle size measurement of the dispersion according to the invention was carried out using a Malvern Mastersizer 2000 (Malvern Instruments GmbH D-Herrenberg; measuring principle: Fraunhofer diffraction in accordance with ISO 13320).
  • a spherical model with a refractive index of the continuous phase of 1.33, a refractive index of the disperse phase of 1.39 and an absorption of 0.01 is assumed as the parameter for the measurement.
  • the measured value is D (50), the median value of the volume distribution.
  • the preparation was carried out analogously to example 1 with the only difference that silicone composition 1 was used.
  • the particle size distribution is monomodal with a D50 value of 300 nm.
  • Dispersion 3A 34.5 g of a 20 wt. aqueous solution of (Y) were placed in a double-walled, water-cooled vessel. 10 g of the silicone composition 3A were added in portions and dispersed with the Ultra-Turrax T50 for a total of 7 minutes at 5000 rpm. This was followed by dilution with 37.9 g of demineralized water by adding in portions and further dispersing at 5000 rpm for a total of 13 minutes. A smooth, white dispersion was obtained. containing 12 wt.% silicone composition, 8 wt.% polyvinyl alcohol and 80% water. The particle size distribution is monomodal with a D50 value of 295 nm.
  • Dispersion 3B was prepared analogously to Dispersion 3A with the only difference that silicone composition 3B was used.
  • the particle size distribution is monomodal with a D50 value of 295 nm.
  • Example 2 The preparation was carried out analogously to Example 1 with the only difference that 1 g of the emulsifier iso-tridecyl alcohol polyglycol ether Genapol® X-080 (CAS No. 9043-30-5, available from Sigma Aldrich) was added to the polyvinyl alcohol solution. A smooth, white dispersion containing 12% silicone composition, 8% polyvinyl alcohol, 1 g emulsifier and 79% water was obtained. The particle size distribution is monomodal with a D50 value of 350 nm.
  • the electrospinning process was carried out analogously to W02014114501.
  • the electrospinning dispersions 1, 2, 4 and 5 are one-component cross-linking and were spun within 24 hours after production.
  • the conditions of the electrospinning system were as follows: Voltage: 22.5 kV direct current Distance between cannula and electrode: 40 cm Diameter of cannula: 1 mm Flow rate: 5 mL/h
  • Aluminum foil was used as the substrate. The electrode was either static or rotated using an electric motor. After the electrospinning process was completed, the sample containing the deposited silicone material and the aluminum foil was photochemically treated using UV radiation or thermally. If silicone composition 2 or 3 (dispersion 1, 3 and 4) was used, the fibers were cured in an oven at 150°C for 20 minutes. If silicone composition 1 or 4 (dispersion 2 and 5) was used, the sample was irradiated for 2 minutes with a mercury vapor lamp (1.5 J/cm 2 ).
  • the deposited material was peeled off the aluminum foil, placed in deionized water (25 °C) and treated with the ultrasonic finger (UP400S, equipped with a sonotrode model S3 with a diameter of 3 mm, maximum amplitude 210 pm; max. sound power density 460 W/cm2 available from Hielscher Ultrasonics GmbH) at 50% amplitude power three times for 5 minutes. Between the passes, the water was exchanged without allowing the fleece to dry out and treated with ultrasound two more times. After this washing step, the sample was washed seven times with deionized water (75 °C).
  • the wet fleece was placed in a Petri dish (diameter 50 mm), covered with deionized water and stored in a freezer at -19°C until the water was frozen.
  • the water was then dried by sublimation in a freeze dryer of the type Epsilon 2-4 LSC (Martin Christ Freeze-Drying Systems GmbH) at increasing temperatures from -40 °C to +20 °C in the form of a temperature staircase with
  • Electrospinning was also carried out analogously as described above.
  • the respective fleece was washed analogously to the examples according to the invention, with the difference that instead of freeze-drying, the sample was dried at 25 °C and normal pressure until constant mass.
  • the obtained nonwoven fabric was examined by SEM.
  • fleeces produced using the non-inventive method the structure of the fiber fleece collapses and its porosity decreases.
  • fleeces produced using the inventive method i.e. dried by sublimation, show an open-pored fiber fleece structure.

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Abstract

La présente invention concerne une solution d'électrofilage à base d'élastomère de silicone et son utilisation pour produire des non-tissés au moyen d'un procédé d'électrofilage amélioré.
PCT/EP2023/068662 2023-07-06 2023-07-06 Dispersion d'électrofilage et procédé de production d'un non-tissé d'élastomère de silicone électrofilé Ceased WO2025008068A1 (fr)

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