EP3655575A1 - Faservliese mit asymmetrischer silica-imprägnierung und verfahren zur herstellung der vliese sowie deren verwendung - Google Patents
Faservliese mit asymmetrischer silica-imprägnierung und verfahren zur herstellung der vliese sowie deren verwendungInfo
- Publication number
- EP3655575A1 EP3655575A1 EP19778972.0A EP19778972A EP3655575A1 EP 3655575 A1 EP3655575 A1 EP 3655575A1 EP 19778972 A EP19778972 A EP 19778972A EP 3655575 A1 EP3655575 A1 EP 3655575A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- fleece
- nonwoven fabric
- weight fraction
- paper
- main surfaces
- 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.)
- Granted
Links
- 239000004745 nonwoven fabric Substances 0.000 title claims abstract description 100
- 238000000034 method Methods 0.000 title claims abstract description 39
- 239000005022 packaging material Substances 0.000 claims abstract description 6
- 238000005470 impregnation Methods 0.000 claims description 100
- 239000000123 paper Substances 0.000 claims description 56
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 50
- 238000001035 drying Methods 0.000 claims description 46
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 37
- 229910000077 silane Inorganic materials 0.000 claims description 37
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 32
- 239000000463 material Substances 0.000 claims description 23
- 239000000377 silicon dioxide Substances 0.000 claims description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 238000004519 manufacturing process Methods 0.000 claims description 11
- 239000007788 liquid Substances 0.000 claims description 6
- 239000012528 membrane Substances 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 239000010902 straw Substances 0.000 claims description 6
- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical compound CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 claims description 6
- -1 polydimethoxysiloxane Polymers 0.000 claims description 4
- 230000003247 decreasing effect Effects 0.000 claims description 3
- 239000003921 oil Substances 0.000 claims description 3
- 238000004806 packaging method and process Methods 0.000 claims description 3
- 238000000926 separation method Methods 0.000 claims description 3
- OTMSDBZUPAUEDD-UHFFFAOYSA-N Ethane Chemical compound CC OTMSDBZUPAUEDD-UHFFFAOYSA-N 0.000 claims description 2
- 239000011088 parchment paper Substances 0.000 claims description 2
- YZVRVDPMGYFCGL-UHFFFAOYSA-N triacetyloxysilyl acetate Chemical compound CC(=O)O[Si](OC(C)=O)(OC(C)=O)OC(C)=O YZVRVDPMGYFCGL-UHFFFAOYSA-N 0.000 claims description 2
- 229910004298 SiO 2 Inorganic materials 0.000 description 22
- 238000009826 distribution Methods 0.000 description 21
- YJHDFAAFYNRKQE-YHPRVSEPSA-L disodium;5-[[4-anilino-6-[bis(2-hydroxyethyl)amino]-1,3,5-triazin-2-yl]amino]-2-[(e)-2-[4-[[4-anilino-6-[bis(2-hydroxyethyl)amino]-1,3,5-triazin-2-yl]amino]-2-sulfonatophenyl]ethenyl]benzenesulfonate Chemical compound [Na+].[Na+].N=1C(NC=2C=C(C(\C=C\C=3C(=CC(NC=4N=C(N=C(NC=5C=CC=CC=5)N=4)N(CCO)CCO)=CC=3)S([O-])(=O)=O)=CC=2)S([O-])(=O)=O)=NC(N(CCO)CCO)=NC=1NC1=CC=CC=C1 YJHDFAAFYNRKQE-YHPRVSEPSA-L 0.000 description 17
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 16
- 238000007654 immersion Methods 0.000 description 14
- 230000002209 hydrophobic effect Effects 0.000 description 11
- 230000008569 process Effects 0.000 description 11
- 239000000835 fiber Substances 0.000 description 9
- 239000002904 solvent Substances 0.000 description 9
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 description 8
- 229940043267 rhodamine b Drugs 0.000 description 8
- 238000001218 confocal laser scanning microscopy Methods 0.000 description 7
- 238000003618 dip coating Methods 0.000 description 7
- 239000013598 vector Substances 0.000 description 7
- 230000005012 migration Effects 0.000 description 6
- 238000013508 migration Methods 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- 238000002411 thermogravimetry Methods 0.000 description 6
- 238000009736 wetting Methods 0.000 description 6
- 238000000576 coating method Methods 0.000 description 5
- 239000002131 composite material Substances 0.000 description 5
- 230000007423 decrease Effects 0.000 description 5
- 238000001704 evaporation Methods 0.000 description 5
- 230000008020 evaporation Effects 0.000 description 5
- 238000005507 spraying Methods 0.000 description 5
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 4
- 230000008901 benefit Effects 0.000 description 4
- 239000011248 coating agent Substances 0.000 description 4
- 239000012530 fluid Substances 0.000 description 4
- 238000005259 measurement Methods 0.000 description 4
- 244000166124 Eucalyptus globulus Species 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 3
- 239000000654 additive Substances 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 230000005661 hydrophobic surface Effects 0.000 description 3
- 238000006116 polymerization reaction Methods 0.000 description 3
- 229920005989 resin Polymers 0.000 description 3
- 239000011347 resin Substances 0.000 description 3
- 239000004698 Polyethylene Substances 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000001913 cellulose Substances 0.000 description 2
- 229920002678 cellulose Polymers 0.000 description 2
- 238000007766 curtain coating Methods 0.000 description 2
- 239000002657 fibrous material Substances 0.000 description 2
- 239000000945 filler Substances 0.000 description 2
- 238000013031 physical testing Methods 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- 229920000573 polyethylene Polymers 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000007761 roller coating Methods 0.000 description 2
- 239000004753 textile Substances 0.000 description 2
- 229920003043 Cellulose fiber Polymers 0.000 description 1
- 229920000426 Microplastic Polymers 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 125000003277 amino group Chemical group 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 239000000560 biocompatible material Substances 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000007859 condensation product Substances 0.000 description 1
- 238000006482 condensation reaction Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000035622 drinking Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000004442 gravimetric analysis Methods 0.000 description 1
- 238000007602 hot air drying Methods 0.000 description 1
- 230000005660 hydrophilic surface Effects 0.000 description 1
- 239000011256 inorganic filler Substances 0.000 description 1
- 150000002561 ketenes Chemical class 0.000 description 1
- 238000010030 laminating Methods 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 239000003550 marker Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000012766 organic filler Substances 0.000 description 1
- 239000013502 plastic waste Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 229920005749 polyurethane resin Polymers 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000005871 repellent Substances 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 238000004513 sizing Methods 0.000 description 1
- 238000010186 staining Methods 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000013517 stratification Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
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
- D21H17/13—Silicon-containing compounds
-
- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/04—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres having existing or potential cohesive properties, e.g. natural fibres, prestretched or fibrillated artificial fibres
- D04H1/26—Wood pulp
-
- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
- D04H1/58—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties by applying, incorporating or activating chemical or thermoplastic bonding agents, e.g. adhesives
- D04H1/587—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties by applying, incorporating or activating chemical or thermoplastic bonding agents, e.g. adhesives characterised by the bonding agents used
-
- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
- D04H1/58—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties by applying, incorporating or activating chemical or thermoplastic bonding agents, e.g. adhesives
- D04H1/64—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties by applying, incorporating or activating chemical or thermoplastic bonding agents, e.g. adhesives the bonding agent being applied in wet state, e.g. chemical agents in dispersions or solutions
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/77—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with silicon or compounds thereof
- D06M11/79—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with silicon or compounds thereof with silicon dioxide, silicic acids or their salts
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M23/00—Treatment of fibres, threads, yarns, fabrics or fibrous goods made from such materials, characterised by the process
- D06M23/16—Processes for the non-uniform application of treating agents, e.g. one-sided treatment; Differential treatment
-
- 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
- D21H17/63—Inorganic compounds
- D21H17/67—Water-insoluble compounds, e.g. fillers, pigments
- D21H17/68—Water-insoluble compounds, e.g. fillers, pigments siliceous, e.g. clays
-
- 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
- D21H19/00—Coated paper; Coating material
- D21H19/36—Coatings with pigments
- D21H19/38—Coatings with pigments characterised by the pigments
- D21H19/40—Coatings with pigments characterised by the pigments siliceous, e.g. clays
-
- 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
- D21H19/00—Coated paper; Coating material
- D21H19/36—Coatings with pigments
- D21H19/44—Coatings with pigments characterised by the other ingredients, e.g. the binder or dispersing agent
- D21H19/46—Non-macromolecular organic compounds
-
- 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
- D21H27/10—Packing paper
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/02—Natural fibres, other than mineral fibres
- D06M2101/04—Vegetal fibres
- D06M2101/06—Vegetal fibres cellulosic
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/10—Repellency against liquids
- D06M2200/12—Hydrophobic properties
Definitions
- the present invention relates to nonwovens with asymmetrical silica impregnation and processes for their production and uses of the nonwovens, in particular in the field of packaging materials.
- composite materials are provided in which there is a modifying layer on the surface of the paper fleece.
- composite materials made of paper and polyethylene are known. These composite materials are obtained by laminating the paper surface with polyethylene films. Layer composites are formed which have hydrophobic surface properties on one side or on both sides. An anisotropic distribution of the chemical impregnation within the paper fleece cannot be achieved with these techniques. In addition, such composite materials are difficult or impossible to recycle (keyword: microplastics). The relatively large amounts of material used for e.g. a coating is required.
- Papers can also be hydrophobized with so-called sizing agents (for example alkylated ketene dimers (AKD)).
- sizing agents for example alkylated ketene dimers (AKD)
- An anisotropic distribution of the chemical impregnation which can also be referred to as asymmetrical distribution, would, however, be associated with many advantages. Functional loading Stratification could be applied in much lower order weights with the same effect. In addition, the targeted adjustment of the material concentration would enable the creation of more complex structures (eg sandwich-like channels in paper) in one process step with minimal use of materials.
- the anisotropic chemical structure results in advantageous property profiles in the nonwovens, for example barrier effects. For example, a fleece could be obtained which cannot be wetted from the outside with fluids (for example water), but which could absorb (and deliver, pass on, and so on ...) the same fluid inside, as well as below described.
- nonwoven fabrics for example paper nonwovens
- the nonwovens are said to be able to be produced by a process which allows the fibers, in particular paper fibers, to be given localized hydrophobic or hydrophilic properties.
- the process should be simple and also allow easy upscaling.
- biocompatible materials are to be obtained.
- the distribution of Si0 2 in the form of a gradient enables one side of the nonwoven, in particular the paper, to absorb water and the other side to repel water, or that both surfaces repel water and water can only be absorbed inside the material. analogous to a chemical sandwich structure.
- the water absorption behavior can be adjusted by adjusting the Si0 2 amount.
- the objects are solved by the subject matter of the claims.
- the objects are achieved in particular by a nonwoven fabric with asymmetrical silica impregnation, the nonwoven having two main surfaces, the weight fraction of SiO 2 decreasing from at least one of the two main surfaces towards the inside of the nonwoven.
- the tasks are also solved by a method for producing a nonwoven fabric with asymmetrical silica impregnation, in particular a nonwoven fabric of the present invention, comprising the following steps: a) providing a nonwoven fabric, b) providing an impregnation solution, the Impregnation solution contains a silane component, c) impregnating the fleece with the impregnation solution, d) drying the fleece at temperatures in a range from 70 ° C. to 190 ° C., a period of at most 60 seconds between the completion of the impregnation according to step c) and the start of drying according to step d).
- the method developed by the inventors preferably uses only a silane component (in particular tetraethylorthosilicate (TEOS), preferably prepolymerized) and a nonwoven fabric, in particular a paper nonwoven, to build up the anisotropic (asymmetrical) impregnation.
- TEOS tetraethylorthosilicate
- the silane component can be inserted into the paper in a simple immersion step. Other impregnation processes are also possible.
- the nonwoven is preferably impregnated with the impregnation solution according to step c) of the method using an impregnation method which is selected from the group consisting of dip coating, spray coating (optionally also on both sides), size press, roller coating, blade coating and curtain coating . Dip coating and spray coating are particularly preferred. Dip coating is very particularly preferred.
- the impregnation solution is preferably distributed uniformly over the surface and the interior of the fleece.
- the silane component produces a silica impregnation in the form of polymeric SiO 2 , which can also be referred to as a silicate component.
- a silicate component This is based not only on drying, but on a chemical reaction taking place at the same time.
- the distribution of the amount of polymeric silicate component is preferably controlled by the drying process, which particularly preferably includes the control of the condensation reaction of the silane component (in particular TEOS) taking place parallel to the drying.
- the location of the impregnation is preferably controlled by the self-diffusion and reactivity of the silane component, which in turn can be easily adjusted via the drying conditions (air humidity, temperature, pressure). It is therefore not necessary to produce a laminate in multiple steps with many additives.
- the process enables the saving of process steps and the amount of material introduced and thus energy and materials based on fossil raw materials.
- the new materials obtainable with the process can be replaced in a variety of ways, for example for hydrophobization in the packaging and food sector.
- the present invention relates to a nonwoven fabric with asymmetrical silica impregnation, where the nonwoven has two main surfaces, the weight fraction of Si0 2 decreasing from at least one of the two main surfaces towards the inside of the nonwoven.
- the nonwoven of the present invention is a nonwoven.
- the nonwoven is preferably selected from the group consisting of paper nonwovens, textile nonwovens and plastic nonwovens.
- the nonwoven is particularly preferably a paper nonwoven.
- the impregnated nonwoven preferably comprises S1O2 in a proportion of 0.1 to 10% by weight, more preferably 0.2 to 7.5% by weight, further preferably 0.5 to 5% by weight.
- the impregnated nonwoven preferably consists of the fiber component (in particular paper) and the impregnation component (SiC> 2).
- the impregnated nonwoven preferably comprises the fiber component in a proportion of 90 to 99.9% by weight, more preferably 92.5 to 99.8% by weight, more preferably 95% to 99.5% % By weight.
- the impregnated nonwoven fabric of the invention preferably consists of the fiber component (in particular special paper) and the impregnation component (S1O2).
- the fleece can contain further components, but preferably in a proportion of at most up to 50% by weight, for example 0 to 30% by weight, more preferably up to 25% by weight, further preferably up to 10 % By weight, more preferably up to 5% by weight, more preferably up to 2% by weight, more preferably up to 1% by weight, more preferably less than 0.5% by weight.
- These further components can in particular be inorganic and / or organic fillers.
- the proportion of the fiber component and impregnation component in the nonwoven of the present invention is preferably at least 50% by weight, more preferably at least 75% by weight, more preferably at least 90% by weight, further preferably at least 95% by weight, further preferably at least 98% by weight, more preferably at least 99% by weight.
- the impregnated nonwoven fabric of the invention preferably consists of the fiber component and the impregnation component.
- the nonwoven of the present invention has an asymmetrical (anisotropic) silica impregnation.
- asymmetrical and “anisotropic” are used synonymously in the present description.
- the silica impregnation is in the form of polymeric Si0 2 , which can also be referred to as a silicate component.
- the silica impregnation is asymmetrical, ie anisotropic. This means that the proportion of Si0 2 is not distributed homogeneously over the fleece, as explained in more detail below.
- the nonwoven of the invention has two major surfaces.
- the length and width of the nonwoven, or in the case of nonwovens with a round base, the diameter of the nonwoven are many times greater than the thickness of the nonwoven.
- the ratio of length and width or diameter of the fleece to the thickness of the fleece is preferably at least 5, more preferably at least 10, more preferably at least 20.
- the shape of the fleece can therefore also be as leaf-like, foil-like, plate-like or disc-like.
- the two main surfaces can also be referred to as the top and bottom or as the front and back of the fleece.
- the weight fraction of SiO 2 decreases from at least one of the two main surfaces towards the interior of the fleece.
- the proportion by weight of Si0 2 is therefore higher on at least one of the two main surfaces than the proportion by weight of Si0 2 below the corresponding main surface.
- the formation of such a Si0 2 gradient brings diverse advantages with it compared to materials with SiO 2 present essentially uniformly distributed over the thickness of the fleece. For example, inner channels and / or different wetting properties of the surfaces can be obtained. In addition, a low use of materials is made possible.
- the weight fraction of SiO 2 on at least one of the two main surfaces is preferably at least 1.1 times as high, more preferably at least twice as high, more preferably at least three times as high, more preferably at least four times as high, more preferably at least five times as high, more preferably at least six times as high, more preferably at least seven times as high, more preferably at least eight times as high, more preferably at least nine times as high, further preferably at least ten times as high as the weight fraction of SiO 2 in the middle of the fleece.
- the center of the fleece designates the positions in the interior of the fleece which are equally far away from the two main surfaces in the shortest possible connection, and which are therefore in the middle of the fleece in relation to the thickness of the fleece.
- the SiO 2 is not only in a gradient distribution in relation to one main surface, but also in relation to the other main surface.
- the gradient does not have to be designed in the same way from both main surfaces to the interior of the fleece.
- the weight fraction of Si0 2 decreases from one of the two main surfaces towards the interior of the fleece, while the weight fraction of Si0 2 increases from the other of the two main surfaces towards the interior of the fleece.
- Such fleeces preferably differ in terms of their properties on the two main surfaces.
- one main surface is significantly more hydrophobic than the other main surface.
- a fleece with a hydrophobic main surface and a hydrophilic main surface is particularly preferred.
- the weight fraction of SiO 2 on one of the two main surfaces is preferably at least 1.1 times as high, more preferably at least two.
- the proportion by weight of S1O2 on the other of the two main surfaces is preferably at most 0.9 times, more preferably at most half, more preferably at most one third, more preferably at most one quarter, more preferably at most one fifth, more preferably at most one Sixth, more preferably at most one seventh, more preferably at most one eighth, more preferably at most one ninth, further preferably at most one tenth of the weight fraction of S1O2 in the middle of the fleece.
- the weight fraction of S1O2 on one of the two main surfaces is preferably at least 1.2 times, more preferably at least 4 times, more preferably at least 10 times, more preferably at least 20 times, further preferably at least 50 times , more preferably at least 100 times the weight fraction of SiO 2 on the other of the two main surfaces.
- the weight fraction of SiO 2 decreases from both main surfaces towards the inside of the fleece.
- Such fleeces preferably do not differ, or do not differ significantly, with regard to their properties on the two main surfaces.
- both main surfaces are hydrophobic.
- a fleece with two hydrophobic main surfaces is particularly preferred. Less material is required compared to a uniform impregnation across the entire thickness of the fleece.
- the proportion by weight of SiO 2 on both main surfaces is preferably at least 1.1 times as high, more preferably at least 1.2 times as high, more preferably at least 1.5 times as high as the proportion by weight of SiO 2 in the middle of the fleece.
- the ratio of the proportion by weight of S1O2 on one main surface to the proportion by weight of S1O2 on the other main surface is in a range from 0.95: 1 to 1.05: 1, more preferably from 0.98: 1 to 1.02 : 1, further preferred from 0.99: 1 to 1, 01: 1.
- the relative Si0 2 distribution in the nonwovens is preferably analyzed with the help of confocal laser scanning microscopy (CLSM, English: "confocal laser scanning microscopy”) on cross sections of embedded samples.
- CLSM confocal laser scanning microscopy
- absolute Si0 2 quantities per fleece which are preferably determined with the help of thermogravimetric analysis (TGA)
- TGA thermogravimetric analysis
- the nonwovens of the invention preferably have a high degree of flexibility.
- the present invention also relates to a method for producing a nonwoven fabric with asymmetrical silica impregnation, in particular a nonwoven fabric of the present invention as described above.
- the invention also relates to a nonwoven fabric with asymmetrical silica impregnation that can be obtained or obtained with the method.
- the method comprises the following steps: a) providing a nonwoven fabric, b) providing an impregnating solution, the impregnating solution containing a silane component, c) impregnating the nonwoven fabric with the impregnating solution, d) drying the nonwoven fabric at temperatures in a range from 70 ° C to 190 ° C, with a period of at most 60 seconds between the completion of the impregnation according to step c) and the start of drying according to step d).
- a nonwoven fabric is provided.
- the nonwoven is preferably selected from the group consisting of paper nonwovens, textile nonwovens and plastic nonwovens.
- the nonwoven is particularly preferably a paper nonwoven.
- the paper fleece provided preferably has a grammage of 65 to 120 g / m 2 , more preferably 70 to 100 g / m 2 , more preferably 75 to 90 g / m 2 .
- the nonwoven can be a commercially available nonwoven.
- the paper fleece can be a commercially available paper fleece.
- the step of providing the nonwoven, in particular the nonwoven can also include the step of producing the nonwoven, in particular the nonwoven.
- a paper fleece is preferably produced using the Rapid-Köthen process, particularly preferably in a Rapid-Köthen sheet-forming system, very particularly preferably in accordance with DIN 54358 and / or ISO 5269/2 (ISO5269-2: 2004 (E), " Pulps - Preparation of Laboratory Sheets for Physical Testing - Part 2: Rapid Köthen Method, 2004 ").
- No further additives or fillers are preferably used in the production of the nonwoven fabric, in particular the paper nonwoven.
- an impregnation solution which contains a silane component.
- the terms “impregnation solution” and “impregnation solution” are used synonymously.
- the impregnation solution can be one component, that is, it can consist of a single component. In such a case, the impregnation solution can in particular also be referred to as “impregnation fluid” or “impregnation fluid”.
- the impregnation solution consists of the silane component.
- the proportion of the silane component in the impregnation solution is 100% by weight.
- the impregnation solution can therefore be pure silane.
- the impregnation solution contains, in addition to the silane component, at least one further component, for example a solvent component and / or an acid component.
- the proportion of the silane component in the impregnation solution is preferably in a range from 5% by weight to 100% by weight, more preferably 10% by weight to 99% by weight, further preferably 20% by weight to 98 % By weight, more preferably 40% by weight to 97% by weight, more preferably 60% by weight to 96% by weight, more preferably 80% by weight to 95% by weight.
- the extent of the water-repellent surface properties of the nonwovens can be specifically adjusted via the proportion of the silane component. Higher proportions of the silane component are associated with more hydrophobic surface properties.
- the silane component is preferably selected from the group consisting of tetraethyl orthosilicate (TEOS), tetramethyl orthosilicate, polydimethoxysiloxane, 1,2-bis (triethoxysilyt) ethane, tetramethyl orthosilicate (TMOS), silicon tetraacetate and mixtures of two or more thereof.
- TEOS tetraethyl orthosilicate
- TMOS tetramethyl orthosilicate
- silicon tetraacetate silicon tetraacetate and mixtures of two or more thereof.
- the silane component TEOS is particularly preferred.
- TEOS is a common basic chemical that is cheap and readily available.
- the silane component is preferably prepolymerized.
- prepolymerized means that only oligomers have already been formed and the material has not yet been polymerized.
- the impregnation solution preferably contains solvents in a proportion which is in a range from 0 to 98% by weight, more preferably from 0.1 to 50% by weight, more preferably from 0.2 to 20% by weight, more preferably from 0.5 to 10% by weight, even more preferably from 1 to 5% by weight.
- the solvent is preferably selected from the group consisting of water, ethanol and mixtures of two or more thereof.
- the solvent is particularly preferably water.
- the impregnation solution preferably contains water in a proportion which is in a range from 0 to 20% by weight, more preferably from 0.5 to 10% by weight, more preferably from 1 to 5% by weight.
- the impregnation solution preferably contains HCl in a proportion of 0.001 to 0.2% by weight, more preferably 0.005 to 0.1% by weight, more preferably 0.01 to 0.05% by weight.
- the impregnation solution according to the invention preferably consists of at least 95% by weight, more preferably at least 98% by weight, more preferably at least 99% by weight, further preferably at least 99.9% by weight, further preferably at least 99.99 % By weight of ethanol, water, silane component and HCl. It is a particular advantage of the method according to the invention that no further components are required in the impregnation solution.
- the impregnation solution is particularly preferably composed of at least 95% by weight, more preferably at least 98% by weight, more preferably at least 99% by weight, more preferably at least 99.9% by weight, more preferably at least 99% 99% by weight of water, silane component and HCl.
- the impregnation solution is preferably stirred for a period of 6 to 48 hours, more preferably from 12 to 36 hours, more preferably from 18 to 30 hours, before the impregnation of the nonwoven fabric, in particular the paper nonwoven, with the impregnation solution according to step c) of the method according to the invention it follows.
- the impregnation solution consists of a silane component (in particular TEOS)
- TEOS preferably no such stirring takes place.
- Step c) of impregnating the nonwoven fabric, in particular the paper nonwoven, with the impregnation solution is preferably carried out at a relative atmospheric humidity in a range from 10% to 95%, more preferably from 30% to 70%, further preferably 40% to 60% , more preferably 45% to 55% and / or at a temperature in a range from 15 ° C to 30 ° C, more preferably 20 ° C to 25 ° C.
- the nonwoven fabric is preferably impregnated with the impregnating solution by exposing the nonwoven to the impregnating solution, in other words by bringing the nonwoven into contact with the impregnating solution.
- the nonwoven fabric is preferably impregnated with the impregnation solution according to step c) of the process using an impregnation process which is selected from the group consisting of dip coating, spray coating (optionally also on both sides), size press, roller coating, blade coating and curtain coating. Dip coating and spray coating are particularly preferred. Dip coating is very particularly preferred.
- the impregnation solution is preferably distributed uniformly over the surface and the interior of the fleece.
- the impregnation in step c) of the invention is carried out by immersing the fleece in the impregnation solution.
- the nonwoven fabric in particular the paper nonwoven, is preferably completely immersed in the impregnation solution.
- the immersion is preferably carried out in such a way that the nonwoven, in particular the nonwoven, is oriented essentially vertically.
- a vertical orientation means that the two main surfaces of the fleece are arranged in such a way that surface vectors perpendicular to the main surfaces are oriented essentially horizontally.
- the surface vectors of the two main surfaces preferably each form an angle of at least 70 ° and at most 110 °, more preferably of at least 80 ° and at most 100 °, more preferably of at least 85 ° and at most 95 °, with the vector of the immersion direction.
- the fleece is preferably removed from the impregnation solution at a point in time which is one to ten seconds, more preferably two to five seconds after the immersion of the fleece in the impregnation solution has ended.
- the fleece is preferably removed from the impregnation solution in such a way that the fleece is oriented essentially vertically.
- a vertical orientation means that the two main surfaces of the fleece are arranged in such a way that surface vectors perpendicular to the main surfaces are oriented essentially horizontally.
- the surface vectors of the two main surfaces preferably form an angle of at least 70 ° and at most 110 °, more preferably of at least 80 ° and at most 100 °, more preferably of at least 85 ° and at most 95 °, with the vector of the distance direction.
- the fleece dries at temperatures in a range from 70 ° C. to 190 ° C.
- the fleece dries at temperatures in a range from 80 ° C. to 180 ° C., more preferably from 90 ° C. to 170 ° C., more preferably from 100 ° C. to 160 ° C., more preferably from 110 ° C. C to 150 ° C, more preferably from 120 ° C to 140 ° C, more preferably from 125 ° C to 135 ° C.
- the fleece is preferably dried in accordance with step d) until the residual moisture of the fleece is in a range from 3% by weight to 7% by weight.
- the residual moisture is preferably determined by means of gravimetric analysis, in particular according to DIN EN 20287.
- step d) of the method according to the invention preferably takes place immediately, in other words immediately, after impregnation of the fleece with the impregnation solution according to step c) of the method.
- the impregnation according to step c) is preferably completed when the nonwoven is no longer exposed to the impregnation solution, or in other words when the nonwoven is no longer brought into contact with the impregnation solution.
- the impregnation according to step c) is preferably completed, for example, when the nonwoven fabric has been completely removed from the impregnation solution again, for example pulled out.
- the impregnation according to step c) is preferably completed, for example, when the fleece is no longer sprayed with the impregnation solution.
- the drying according to step d) preferably begins when the fleece comes into an environment which is intended to remove moisture and / or condensation products, for example in an oven.
- the short period between completion of the impregnation and the beginning of the drying probably means that the silane component of the impregnation solution has not yet been converted to a substantial extent into the silicate component of the silica impregnation if the drying at the increased Drying temperatures occur.
- This enables the targeted adjustment of the asymmetrical silica impregnation. This is because the silane component migrates through the fleece at the elevated drying temperatures depending on the drying conditions, in particular the ambient pressures, as long as it has not yet been converted into an overly polymerized silica impregnation.
- the migration of the silane component through the fleece at the elevated drying temperatures can be influenced, in particular, by adjusting the ambient pressures during drying.
- the migration of the silane component can in particular also be influenced by the evaporation of the silane component and / or the solvent at the elevated drying temperatures, since the silane component passes through with the solvent the fleece wanders.
- the method of the present invention provides that between the completion of the impregnation according to step c) and the start of drying according to step d) there is a period of at most 60 seconds. Extensive polymerization has therefore not yet taken place at the start of drying, so that the silane component present in the impregnation solution migrates through the fleece and the distribution of the silica impregnation can therefore be influenced in a targeted manner via the migration.
- nonwovens with asymmetrical silica impregnation can be obtained be formed such that the SiC weight fraction on one main surface is higher than in the middle of the fleece, while the SiO 2 weight fraction on the other main surface is lower than in the middle of the fleece.
- non-woven fabrics can be obtained with an asymmetrical silica impregnation which is designed such that the Si0 2 weight fraction on both main surfaces is approximately the same, namely higher than in the middle of the fleece, since the silane component migrates from the center towards the main surfaces and then there is an increased formation of the polymeric silica Impregnation is coming.
- Drying is preferably carried out with the aid of a dryer.
- the dryer is preferably selected from the group consisting of hot air dryers, ovens, drum dryers and IR dryers.
- drying can be carried out in an oven, preferably in a vacuum oven or in a muffle oven.
- the oven is preferably preheated, in particular to the drying temperature, so that after the impregnation in step c), drying in step d) can be started particularly quickly.
- the dryer is particularly preferably a hot air dryer. Hot air drying is particularly preferred.
- the properties of the nonwovens obtained can be influenced not only by the process steps described above, but in particular also by the ambient pressure prevailing during drying.
- Nonwovens with comparatively high Si0 2 contents on both main surfaces can be obtained in particular at low pressures.
- the pressure during the drying according to step d) is preferably in a range from 0.1 kPa to 500 kPa, more preferably from 0.2 kPa to 200 kPa. In certain preferred embodiments, the pressure during the drying according to step d) is in a range from 0.1 kPa to 30 kPa, more preferably from 0.2 kPa to 20 kPa, more preferably from 0.5 kPa to 10 kPa, more preferably from 1 kPa to 5 kPa.
- Such embodiments are particularly suitable for the production of such nonwovens in which the SiC> 2 content on both main surfaces is comparatively high, but is comparatively low in the middle of the nonwoven (so-called sandwich structure).
- the pressure during the drying according to step d) is in a range from> 30 kPa to 500 kPa, more preferably from 50 kPa to 200 kPa, more preferably from 60 kPa to 150 kPa, more preferably from 70 kPa to 130 kPa, more preferably from 80 kPa to 120 kPa, more preferably from 90 kPa to 110 kPa.
- Such embodiments are particularly suitable for the production of those nonwovens in which the SiO 2 content on one of the two main surfaces is significantly higher than on the other of the two main surfaces, while the content of S1O2 in the middle of the nonwoven is less than one of the two main surfaces, but higher than the other of the two main surfaces.
- the nonwovens are preferably arranged essentially horizontally or oriented horizontally.
- a horizontal orientation means that the two main surfaces of the fleece are arranged in such a way that surface vectors perpendicular to the main surfaces are oriented essentially vertically.
- the nonwovens are preferably cooled to a temperature of from 15 ° C. to 30 ° C., more preferably from 20 ° C. to 25 ° C.
- the method preferably consists of the specified steps. It is a particular advantage of the method according to the invention that the method requires very few steps.
- the present invention also relates to the use of a nonwoven of the present invention, in particular as packaging material.
- Preferred uses as packaging material include the use as frozen paper, the use for products that come into contact with food, such as (paper) cups and / or (paper) straws, and the use as packaging for mate- rialien that are protected from liquid, but should still exchange moisture.
- the nonwovens of the present invention can be used for plastic-free straws and / or paper cups. Against the background of possible regulations for the reduction of plastic waste, it can be assumed that there will be an increased demand for plastic-free products. Nonwovens for the uses mentioned, in particular for use in drinking straws and cups, are often also referred to as special papers.
- Embodiments in which the SiCV content on one of the two main surfaces is significantly higher than on the other of the two main surfaces are particularly suitable for use as paper cups.
- the main surface with the higher Si0 2 content is suitable because of its hydrophobicity as the inside of the cup, because the hydrophobic properties of the surface prevent excessive entry of the liquid in the cup into the interior of the fleece.
- the more hydrophilic surface works well as the outer surface of the cup because it promotes printability.
- Embodiments are particularly suitable for use as a straw in which the SiO 2 content on both main surfaces is comparatively high, but is comparatively low in the middle of the fleece (so-called sandwich structure).
- the high Si0 2 content on the two main surfaces prevents excessive liquid from entering the interior of the fleece.
- the fact that the Si0 2 content in the middle of the fleece is comparatively low enables material to be saved.
- the present invention also relates to the use of a nonwoven of the present invention as a membrane, in particular as a membrane for water / oil separation.
- a membrane can be used in particular for the spatial separation of mixtures consisting of a liquid, hydrophobic component (in particular oil) and water.
- the present invention also relates to the use of a nonwoven of the present invention as special paper for use at elevated temperatures, in particular the use of a nonwoven of the present invention as baking paper. Description of the figures
- FIG. 1 shows schematically the evaporation from the nonwovens (1) when drying under normal pressure (FIG. 1A) or in a vacuum (FIG. 1B).
- Under normal pressure there was a high evaporation rate (2) on the top (illustrated by the longer arrows) and a low evaporation rate (3) on the underside of the fleece (1) (illustrated by the shorter arrows).
- In the vacuum there is an average evaporation rate on the top and bottom (4).
- FIG. 2 shows schematically the fluorescence intensity (y-axis) of rhodamine B over the thickness of the fleeces (x-axis).
- the distribution is schematically sketched for non-woven fabrics dried under normal pressure in FIG. 2A and for non-woven fabrics dried in a vacuum in FIG. 2B.
- the location of the two main surfaces ("main sides") is given for orientation.
- the sketch shows an exemplary fluorescence distribution in nonwoven fabrics with an asymmetrical silica impregnation, which is designed in such a way that the Si0 2 weight fraction on one main surface is higher than in the middle of the nonwoven, while the Si0 2 -
- the proportion by weight of the other main surface is less than that in the middle of the fleece (FIG. 2A) and in the case of non-woven fabrics with an asymmetrical silica impregnation which is designed such that the SiO 2 proportion by weight on both main surfaces is approximately the same , namely higher than in the middle of the fleece ( Figure 2B).
- Eucalyptus sulfate fiber (“curl”: 16.2%; degree of fiberization: 1.3%; fine fraction: 15.2%) was used to produce a paper fleece.
- the fibrous material was ground in a Voith LR 40 laboratory refiner. It was milled with an effective specific energy of 16 kWh / t (750,000 revolutions).
- Paper fleeces with a grammage of 80 ⁇ 0.9 g / m 2 were made from the eucalyptus sulfate fibrous material using a Rapid-Köthen sheet formation system in accordance with DIN 54358 and ISO 5269/2 (ISO5269-2: 2004 (E), "Pulps - Preparation of Laboratory Sheets for Physical Testing - Part 2: Rapid Köthen Method, 2004"). No additives or fillers were used. 2. Production of the Si0 2 paper hybrid materials
- the solutions contained TEOS, ethanol (EtOH), water (H2O) and HCl in the following molar ratios:
- Thermogravimetric analysis was carried out with a TGA 1 (Mettler-Toledo). The samples were heated from 25 ° C to 600 ° C at a rate of 10 ° C / min under a constant air flow of 30 ml / min. With these measurements it is possible to determine the content of S1O2, since S1O2 is stable up to temperatures of 1700 ° C.
- the proportion of Si0 2 in the Si0 2 paper hybrid materials is therefore about 0.6% by weight for the nonwovens obtained by treatment with the low-concentration TEOS solution and about 4% by weight for the Nonwovens obtained by treatment with the highly concentrated TEOS solution.
- Nonwovens were made as described in Examples 1 and 2. However, before treatment with the TEOS solution for producing the hybrid materials according to Example 2, the dye Calcofluor White (CFW) was introduced into the nonwovens in the following manner:
- Paper webs from Example 1 were immersed in a CFW solution containing 10 mM CFW in ethanol (absolute) and then dried at 40 ° C. in a vacuum oven for one hour. This staining will later serve as a reference, since CFW is homogeneously distributed over the paper nonwovens due to the high binding affinity for cellulose and does not migrate during drying.
- the nonwovens labeled in this way were treated with TEOS solutions and dried as described in Example 2, the immersion solutions additionally containing 20 mM Rhodamine B. hb) production of the cross sections
- Each sample was embedded in a mixture of 49.9875% by weight Desmodur 3200, 49.9875% by weight Albodur 956 VP and 0.025% by weight TIB-KAT 318.
- the mixture is a commercial polyurethane system.
- the freshly embedded samples were subjected to several vacuum cycles at room temperature in order to remove remaining air bubbles.
- the resin was then cured at 80 ° C for 18 hours.
- samples with a thickness of 120 ⁇ m were cut.
- the section plane was chosen so that it is oriented orthogonally to both main surfaces.
- the samples were placed between two 25 mm round microscope coverslips using Leica Type F immersion liquid.
- the images were taken on a Leica TCS SP8.
- a lens of the type "HC PL APO CS2 20x / 0.75 IMM" in water immersion was used, CFW was excited with a 405 nm laser and detected at 415-557 nm.
- Rhodamine B was excited with a 552 nm laser and detected at 562-753 nm.
- CFW serves as a reference value.
- CFW has a high affinity for cellulose and is therefore evenly distributed over the entire thickness of the fleece. If the CFW fluorescence value fluctuates significantly across the paper cross-section, this can indicate problems in the beam path (such as air pockets), since CFW is physically homogeneously distributed on the paper.
- SiO 2 layer thicknesses it can happen that amino groups of CFW react with the polyurethane resin, whereby the fluorescence of CFW is deactivated.
- S1O2 there is no reaction with the resin, so that the fluorescence is retained.
- Rhodamine B serves as a ratiometric marker for the proportion of Si0 2 .
- RhoB fluorescence the higher the RhoB fluorescence, the higher the proportion of Si0 2 .
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- Dispersion Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
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Abstract
Description
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DE102018124255.7A DE102018124255A1 (de) | 2018-10-01 | 2018-10-01 | Faservliese mit asymmetrischer Silica-Imprägnierung und Verfahren zur Herstellung der Vliese sowie deren Verwendungen |
PCT/EP2019/075927 WO2020069943A1 (de) | 2018-10-01 | 2019-09-25 | Faservliese mit asymmetrischer silica-imprägnierung und verfahren zur herstellung der vliese sowie deren verwendung |
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EP4311875A1 (de) * | 2022-07-27 | 2024-01-31 | Technische Universität Darmstadt | Mit siliciumdioxid beschiteter vliesstoff, verfahren zu seiner herstellung sowie seine verwendung |
EP4311872A1 (de) * | 2022-07-27 | 2024-01-31 | Technische Universität Darmstadt | Nassfestigkeitsverbesserte faservliese, insbesondere papier, verwendung dieser nassfestigkeitsfliese sowie herstellungsverfahren dafür |
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US3551272A (en) * | 1967-05-09 | 1970-12-29 | Monsanto Co | Paper overlays and laminated materials |
US3944702A (en) * | 1974-06-24 | 1976-03-16 | Dow Corning Corporation | Fibrous structures bonded with a silsesquioxane-containing composition |
GB2045823B (en) * | 1979-04-09 | 1983-04-20 | Beloit Corp | Water repellency of a cellulosic web |
US4469746A (en) * | 1982-06-01 | 1984-09-04 | The Procter & Gamble Company | Silica coated absorbent fibers |
JPH0717085B2 (ja) * | 1987-11-20 | 1995-03-01 | キヤノン株式会社 | 記録紙及びこれを用いたインクジェット記録方法 |
US4789564A (en) * | 1987-03-31 | 1988-12-06 | Union Carbide Corporation | Hydridoaminosilane treatment for rendering surfaces water-repellent |
ATE282729T1 (de) * | 2000-09-06 | 2004-12-15 | Toray Industries | Hitzebeständiges gewebe und dessen herstellungsverfahren |
US20040084164A1 (en) * | 2002-11-06 | 2004-05-06 | Shannon Thomas Gerard | Soft tissue products containing polysiloxane having a high z-directional gradient |
EP1944351A1 (de) * | 2007-01-12 | 2008-07-16 | Nederlandse Organisatie voor Toegepast-Natuuurwetenschappelijk Onderzoek TNO | Als Flammenhemmer geeignete Zusammensetzungen |
SE534210C2 (sv) * | 2009-10-09 | 2011-05-31 | Stora Enso Oyj | Process för tillverkning av ett substrat innehållande kiseldioxidpigment som bildas på ytan av substratet |
JP2011162756A (ja) * | 2010-02-15 | 2011-08-25 | Eiju Sangyo:Kk | 多孔質シリカ−繊維複合体の製造方法、多孔質シリカ−繊維複合体およびそれを用いた真空断熱材 |
CN103628351A (zh) * | 2013-11-11 | 2014-03-12 | 华南理工大学 | 一种应用氯硅烷制备超疏水纸张的方法 |
KR20160101330A (ko) * | 2015-02-16 | 2016-08-25 | 알이엠텍 주식회사 | 미세 분말 함침 부직포 및 이의 제조 방법 |
CN106187069A (zh) * | 2016-07-06 | 2016-12-07 | 天津大学 | 一种超疏水轻质高强隔热材料的制备方法 |
CN106283204A (zh) * | 2016-08-17 | 2017-01-04 | 张静 | 一种抗菌无胶棉的制备方法 |
US10762888B2 (en) * | 2017-02-13 | 2020-09-01 | Hyundai Motor Company | Sound absorbing fabric with improved thermal insulation and method of manufacturing the same |
CN108411707A (zh) * | 2018-01-23 | 2018-08-17 | 天津大学 | 一种超亲油及超疏水性油水分离滤纸及其制备方法 |
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2018
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2019
- 2019-09-25 US US17/281,398 patent/US20220034041A1/en active Pending
- 2019-09-25 EP EP19778972.0A patent/EP3655575B1/de active Active
- 2019-09-25 CN CN201980064703.1A patent/CN112840073B/zh active Active
- 2019-09-25 WO PCT/EP2019/075927 patent/WO2020069943A1/de unknown
Also Published As
Publication number | Publication date |
---|---|
EP3655575B1 (de) | 2021-08-25 |
DE102018124255A1 (de) | 2020-04-02 |
US20220034041A1 (en) | 2022-02-03 |
WO2020069943A1 (de) | 2020-04-09 |
CN112840073A (zh) | 2021-05-25 |
CN112840073B (zh) | 2023-04-11 |
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