EP3274502A1 - Paper containing synthetic fibres - Google Patents
Paper containing synthetic fibresInfo
- Publication number
- EP3274502A1 EP3274502A1 EP16711006.3A EP16711006A EP3274502A1 EP 3274502 A1 EP3274502 A1 EP 3274502A1 EP 16711006 A EP16711006 A EP 16711006A EP 3274502 A1 EP3274502 A1 EP 3274502A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- fibers
- paper
- synthetic fibers
- form factor
- paper according
- 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
- 229920002994 synthetic fiber Polymers 0.000 title claims abstract description 105
- 239000000835 fiber Substances 0.000 claims description 153
- 239000012209 synthetic fiber Substances 0.000 claims description 101
- 239000004952 Polyamide Substances 0.000 claims description 21
- 229920002647 polyamide Polymers 0.000 claims description 21
- -1 polyethylene Polymers 0.000 claims description 21
- 239000004698 Polyethylene Substances 0.000 claims description 16
- 229920000573 polyethylene Polymers 0.000 claims description 16
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 11
- 229920000139 polyethylene terephthalate Polymers 0.000 claims description 11
- 239000005020 polyethylene terephthalate Substances 0.000 claims description 11
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 11
- 238000004519 manufacturing process Methods 0.000 claims description 10
- 239000004816 latex Substances 0.000 claims description 6
- 229920000126 latex Polymers 0.000 claims description 6
- 229920000219 Ethylene vinyl alcohol Polymers 0.000 claims description 5
- 229920006149 polyester-amide block copolymer Polymers 0.000 claims description 5
- 239000003795 chemical substances by application Substances 0.000 claims description 4
- 229920000098 polyolefin Polymers 0.000 claims description 4
- 238000010494 dissociation reaction Methods 0.000 claims description 3
- 230000005593 dissociations Effects 0.000 claims description 3
- 239000004715 ethylene vinyl alcohol Substances 0.000 claims description 3
- 229920001577 copolymer Polymers 0.000 claims 1
- RZXDTJIXPSCHCI-UHFFFAOYSA-N hexa-1,5-diene-2,5-diol Chemical compound OC(=C)CCC(O)=C RZXDTJIXPSCHCI-UHFFFAOYSA-N 0.000 claims 1
- 239000000203 mixture Substances 0.000 abstract description 28
- 239000000123 paper Substances 0.000 description 86
- 239000000758 substrate Substances 0.000 description 62
- 238000000034 method Methods 0.000 description 19
- 229920000728 polyester Polymers 0.000 description 11
- 238000005452 bending Methods 0.000 description 8
- 229920003023 plastic Polymers 0.000 description 8
- 239000004033 plastic Substances 0.000 description 8
- 239000002131 composite material Substances 0.000 description 7
- 239000004743 Polypropylene Substances 0.000 description 6
- 239000004745 nonwoven fabric Substances 0.000 description 6
- 229920001155 polypropylene Polymers 0.000 description 6
- 239000011230 binding agent Substances 0.000 description 5
- 239000000945 filler Substances 0.000 description 5
- 229920000642 polymer Polymers 0.000 description 5
- 238000009877 rendering Methods 0.000 description 5
- 125000000129 anionic group Chemical group 0.000 description 4
- 125000002091 cationic group Chemical group 0.000 description 4
- 239000006185 dispersion Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000000700 radioactive tracer Substances 0.000 description 4
- 229920005989 resin Polymers 0.000 description 4
- 239000011347 resin Substances 0.000 description 4
- OVSKIKFHRZPJSS-UHFFFAOYSA-N 2,4-D Chemical compound OC(=O)COC1=CC=C(Cl)C=C1Cl OVSKIKFHRZPJSS-UHFFFAOYSA-N 0.000 description 3
- 229920000508 Vectran Polymers 0.000 description 3
- 239000004979 Vectran Substances 0.000 description 3
- 125000003118 aryl group Chemical group 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 238000001125 extrusion Methods 0.000 description 3
- 238000009472 formulation Methods 0.000 description 3
- 230000003993 interaction Effects 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 229920001909 styrene-acrylic polymer Polymers 0.000 description 3
- 239000004962 Polyamide-imide Substances 0.000 description 2
- 239000000783 alginic acid Substances 0.000 description 2
- 239000001913 cellulose Substances 0.000 description 2
- 229920002678 cellulose Polymers 0.000 description 2
- 238000003776 cleavage reaction Methods 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 230000000593 degrading effect Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000004049 embossing Methods 0.000 description 2
- 230000005284 excitation Effects 0.000 description 2
- 239000008394 flocculating agent Substances 0.000 description 2
- 238000005470 impregnation Methods 0.000 description 2
- 238000003780 insertion Methods 0.000 description 2
- 230000037431 insertion Effects 0.000 description 2
- 229920002312 polyamide-imide Polymers 0.000 description 2
- 229920002635 polyurethane Polymers 0.000 description 2
- 239000004814 polyurethane Substances 0.000 description 2
- 239000012783 reinforcing fiber Substances 0.000 description 2
- 230000007017 scission Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000000725 suspension Substances 0.000 description 2
- 229920001059 synthetic polymer Polymers 0.000 description 2
- KKEYFWRCBNTPAC-UHFFFAOYSA-L terephthalate(2-) Chemical compound [O-]C(=O)C1=CC=C(C([O-])=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-L 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000004448 titration Methods 0.000 description 2
- 238000011282 treatment Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 238000004438 BET method Methods 0.000 description 1
- 229920000742 Cotton Polymers 0.000 description 1
- BRLQWZUYTZBJKN-UHFFFAOYSA-N Epichlorohydrin Chemical compound ClCC1CO1 BRLQWZUYTZBJKN-UHFFFAOYSA-N 0.000 description 1
- 229920002873 Polyethylenimine Polymers 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000011149 active material Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000002671 adjuvant Substances 0.000 description 1
- 239000007767 bonding agent Substances 0.000 description 1
- 239000011111 cardboard Substances 0.000 description 1
- 206010061592 cardiac fibrillation Diseases 0.000 description 1
- 238000009960 carding Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000008119 colloidal silica Substances 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000010101 extrusion blow moulding Methods 0.000 description 1
- 230000002600 fibrillogenic effect Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 239000011121 hardwood Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229920001903 high density polyethylene Polymers 0.000 description 1
- 239000004700 high-density polyethylene Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 150000003949 imides Chemical class 0.000 description 1
- 230000000977 initiatory effect Effects 0.000 description 1
- 238000009940 knitting Methods 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000011087 paperboard Substances 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 229920002401 polyacrylamide Polymers 0.000 description 1
- 229920000058 polyacrylate Polymers 0.000 description 1
- 239000002491 polymer binding agent Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 239000004800 polyvinyl chloride Substances 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000004826 seaming Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000009987 spinning Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 238000003856 thermoforming Methods 0.000 description 1
- 229920001169 thermoplastic Polymers 0.000 description 1
- 239000012815 thermoplastic material Substances 0.000 description 1
- 239000004416 thermosoftening plastic Substances 0.000 description 1
- 238000009732 tufting Methods 0.000 description 1
- 238000009941 weaving Methods 0.000 description 1
- 239000002023 wood Substances 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
- D21H13/00—Pulp or paper, comprising synthetic cellulose or non-cellulose fibres or web-forming material
- D21H13/10—Organic non-cellulose fibres
-
- 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
- D21H13/00—Pulp or paper, comprising synthetic cellulose or non-cellulose fibres or web-forming material
- D21H13/10—Organic non-cellulose fibres
- D21H13/12—Organic non-cellulose fibres from macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H13/00—Pulp or paper, comprising synthetic cellulose or non-cellulose fibres or web-forming material
- D21H13/10—Organic non-cellulose fibres
- D21H13/20—Organic non-cellulose fibres from macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D21H13/24—Polyesters
-
- 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
- D21H13/00—Pulp or paper, comprising synthetic cellulose or non-cellulose fibres or web-forming material
- D21H13/10—Organic non-cellulose fibres
- D21H13/20—Organic non-cellulose fibres from macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D21H13/26—Polyamides; Polyimides
-
- 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
- D21H15/00—Pulp or paper, comprising fibres or web-forming material characterised by features other than their chemical constitution
- D21H15/02—Pulp or paper, comprising fibres or web-forming material characterised by features other than their chemical constitution characterised by configuration
Definitions
- the present invention relates to fibrous documents, including secure documents.
- the invention relates more particularly but not exclusively to a paper suitable for producing secure documents and to its manufacturing process.
- “Secure document” means a security or valuable document, such as a means of payment, for example a bank note, a check, a bank card or a restaurant ticket, an identity document, such as an identity card, a visa, a passport, including the personal data page of a passport, an inlay or a driving license, a lottery ticket, a ticket or an entry ticket to cultural or sporting events.
- a document substrate security elements, for example in the form of fibers, boards, films, knitted structures or security threads.
- the document substrate may itself be made of a material that is difficult to counterfeit, and is then referred to as a "safety substrate".
- cellulosic substrates so-called “composite” substrates, plastic substrates and so-called “hybrid” substrates are known.
- Cellulosic substrates are fibrous substrates generally obtained by the papermaking process, also called wet process, from cellulosic fibers such as hardwood fibers, coniferous fibers, annuals, especially cotton, or their mixtures.
- papermaking or “wet process” is meant a common papermaking process, including in particular the following successive steps:
- composite substrates are cellulosic substrates whose fibrous composition comprises, in addition to the cellulosic fibers, synthetic fibers. Such fibers are generally introduced at levels of less than 20% by dry weight relative to the total weight of the substrate, and their use makes it possible to increase the mechanical strength of the substrate.
- cellulosic fibers plays an important role in the entanglement and fixation of synthetic fibers, which makes it possible to reveal the intrinsic potential of synthetic fibers. Indeed, in the development of the mechanical performance of a sheet material, the performance of the polymer of the synthetic fibers are important but the ability of interaction of the fibers between them is also critical. The presence of refined cellulosic fibers greatly favors the bridging between the cellulose and the polymer of the synthetic fibers.
- Composite substrates have better resistance to circulation than cellulosic substrates.
- resistance to circulation denotes the combination of the following properties: bending resistance, tear resistance and resistance to soiling.
- hybrid substrates comprise at least one cellulosic or composite substrate associated with at least one plastic layer. With respect to the cellulosic or composite substrate that composes them, they generally exhibit equivalent tear resistance and improved bending resistance.
- Hybrid substrates used in the field of security substrates are described in particular in applications WO 2006/066431, WO 2004/028825, EP 1 854 641, WO 03/054297 and WO 94/29105.
- Plastic substrates are conventionally obtained by extrusion of a polymer. These substrates are normally of "very high durability”.
- plastic substrates are especially described in applications EP 2 225 102, WO 99/67093, WO 97/01438 and WO 83/00659. These substrates have good resistance to bending and soiling, but their resistance to tear initiation is relatively low.
- nonwoven substrate is defined in ISO 9092 and EN 29092 as being a manufactured sheet, consisting of a directionally or randomly oriented fiber web or web, bonded by friction and / or cohesion, and / or adhesion , excluding paper and products obtained by weaving, knitting, tufting or seaming, incorporating binding yarn or filament or felts by wet embossing, whether or not needle punched.
- the nonwovens are described as being able to be used as safety substrates in the applications WO 2002/38368 and FR 2 447 995.
- These substrates generally consist of long non-cellulosic fibers, for example of length between 3 and 25 mm. , and have a high mass volume and porosity, which gives them a low resistance to soiling.
- the nonwovens are manufactured according to various processes, especially in the dry process, for example by carding or aerodynamic process (also called “Airlaid”), in the melted process, especially by extrusion (also called “Spunbond”) or extrusion blow molding (also called “Meltblown”), wet (also called “Wetlaid”) according to a process similar to the paper process, or in other ways, including dissolution in a solvent (also called “Flash spinning”).
- Nonwovens made in the wet process generally comprise cellulosic fibers, for example at least 10%, especially in order to ensure better cohesion to the substrate obtained. Moreover, when the proportion of cellulosic fibers in the nonwovens made in the wet process is low or even zero, the hydrogen bonds formed between these fibers do not make it possible to ensure sufficient cohesion to the substrate and it is therefore necessary to at least one bonding step. Such a bond can be achieved by impregnation, spraying or coating of latex, by thermo-fixing, by needling or by water jet bonding (also called "Spunlace").
- the mechanical properties of a paper can also be improved by introducing into the mass of it reinforcing fibers.
- These reinforcing fibers are generally introduced at a rate of more than 3% by dry weight, relative to the total mass by dry weight of the paper fibers, and are most often based on synthetic polymers type polyamide 6.6 (PA 6.6) or polyethylene terephthalate (PET) for the mechanical strength that these polymers confer and for economic reasons, manufacturing and good interaction with the cellulosic fibers of the paper.
- PA 6.6 polyamide 6.6
- PET polyethylene terephthalate
- synthetic fibers By “synthetic fibers”, it is necessary to understand fibers made with one or more synthetic polymers, which are polymers obtained from a chemical synthesis, in particular by a polymerization reaction of monomers, coupled or not to a crosslinking reaction.
- the unsplit synthetic fibers have a number average length of between 0.5 and 8 mm, better 2 and 8 mm, and even more preferably 4 and 6.5 mm.
- Such a paper is also compatible with the main security measures implemented for the papers, especially the watermarking and the insertion, at least partially in mass, of security threads.
- the present inventors have found that synthetic fibers, although having a significant contribution to sheet formation and watermark rendering, have a limited contribution to improving strength properties.
- the Applicant has also found that the unsfabricated synthetic fibers, although having a significant contribution in terms of improving the strength properties, have a negative influence on the hand (mass volume) of the paper and rendering the watermark.
- the invention aims to meet this need, and it achieves this through a paper, comprising:
- unshaped synthetic fibers of section having a second form factor, greater than the first.
- the two form factors differ preferably by a factor of at least two.
- the first form factor may be close to 1, which corresponds to fibers of substantially circular cross section.
- the second form factor may be greater than 2, more preferably 3, more preferably 5 or 10, which corresponds to fibers of flattened cross section, in particular substantially rectangular.
- the substrate according to the invention is a paper, which means that it is obtained by papermaking, in particular according to an inclined table method, flat table and / or round shape. It is preferably a round shape process, for example to obtain a better definition of watermark or to incorporate, at least partially in mass, a security thread.
- the techniques conventionally used to secure the papers can thus be used to secure the substrate according to the invention.
- the substrate according to the invention has improved properties compared with cellulosic papers, in particular an upper tear resistance.
- Fibrillated fibers are fibers with fibrils, i.e., extensions that deviate from the body of the fiber.
- the fibrillated fibers may in particular be fibers in which at least one wall has been partially broken off, causing the partial release of fibrils.
- Such fibers are branched by the fibrils, the section of which is much smaller than that of the fiber as a whole, which increases the interaction of these fibers with the other fibers, in particular synthetic fibers, and limits the ability of the fibers to slip the fibers. one against the other.
- Such fibers are described for example in documents FR1317778 and FR2199015.
- the fibrillated fibers therefore play an important role in the cohesion of a paper according to the invention, in particular by entanglement effects.
- the paper according to the invention can comprise synthetic fibers which are fibers which are fibers of polyamide (PA), polyethylene (PE), polypropylene (PP), poly (ethylene terephthalate) (PET, also called polyester), polyvinyl alcohol (PVA), aromatic polyester (e.g., Vectran ® sold by Kuraray), polyamide imide, polyolefin, and preferably polyacrylic fibers, for example such as those marketed by the company under the reference Sterling CFF 111-2.
- the material of the synthesized fibers has a tensile strength of between 300 and 600 MPa.
- the presence of the synthetic fibers frayed in the invention overcomes the absence or the lower amount of cellulosic fibers, and provides the desired mechanical performance in terms of resistance to tearing and bending.
- the paper comprises fibers made of polyethylene, especially high density polyethylene. Indeed, in addition to their ease of implementation, these fibers make it possible to obtain a good rendering of watermark.
- the proportion of fibrillated fibers of polyethylene is preferably greater than 50% by dry weight relative to the total dry weight of the fibers.
- the average length of the fibrillated fibers of polyethylene is preferably between 0.5 and 2 mm.
- the fibrous composition of the paper comprises at least 20%, preferably at least 50%, by dry weight of fibrillated fibers of polyethylene, it is also possible:
- the other components of the paper generally having melting temperatures higher than the latter.
- the synthetic fibrilated fibers have an average length of between 0.5 mm and 8 mm, preferably between 2 mm and 8 mm and better still between 4 and 6.5 mm.
- the specific surface area of the synthetic fibers which are screened according to the invention is preferably between 35 and 75 m 2 / g, more preferably around 50 m 2 / g. She is measured according to ISO 9277 "Determination of the mass area (specific surface area) of solids by gas adsorption - BET method".
- the paper according to the invention comprises more than 5% by dry weight, better still more than 10% by dry weight and more preferably more than 20% by dry weight, of synthetic fibers fibrillated with respect to the total weight of the paper.
- the paper according to the invention comprises more than 50% by dry weight of fibrillated synthetic fibers relative to the total weight of the paper
- the fibrillated synthetic fibers may be white or colored, in particular of a color that may be the same or different from that (s) of other synthetic fibers.
- the level of fibrillation of the fibers may be between 5 and 700 ml and preferably between 5 and 100 ml according to the CSF standard.
- the fibers may contain at least one tracer, said tracer for identifying the fibers by a specific means, in particular by exposure to UV and / or IR radiation and / or by exposure to a chemical developer.
- This tracer can thus be a luminescent tracer, especially fluorescent under UV or IR.
- the fibrillated fibers may not all have the same formulation.
- Non-fibrillated synthetic fibers having a first shape factor section, in particular with a substantially circular section
- the form factor of these fibers is less than 1.5, more preferably less than or equal to 1.3, more preferably 1.1, which corresponds to a substantially circular section.
- the form factor is defined as the ratio of the largest external dimension in cross-section to the smallest external dimension in the same section.
- a fiber of perfectly circular section thus has a form factor equal to 1.
- An oval section fiber of low eccentricity may have a form factor close to 1.
- the form factor is equal to ratio of the width of the section to its thickness.
- the form factor is equal to 2 1/2 .
- the non-fibrillated synthetic fibers of first form factor are preferably chosen from polyamide (PA), polyacrylic, polypropylene (PP) and poly (ethylene terephthalate) fibers (PET, also known as polyester), polyvinyl alcohol (PVA), aromatic polyester (e.g. Vectran marketed by Kuraray), polyamide imide, ethylene vinyl alcohol copolymer (EVOH), polyolefin and preferably polyethylene (PE).
- PA polyamide
- PP polyacrylic
- PET poly (ethylene terephthalate) fibers
- PVA polyvinyl alcohol
- aromatic polyester e.g. Vectran marketed by Kuraray
- polyamide imide ethylene vinyl alcohol copolymer
- EVOH ethylene vinyl alcohol copolymer
- PE polyolefin and preferably polyethylene
- non-fibrillated synthetic fibers are more preferably polyamide fibers, among other thermoplastic fibers.
- the paper according to the invention preferably comprises less than 95% by dry weight, better less than 90% by dry weight and more preferably less than 80% by dry weight of such non-fibrillated synthetic fibers of first form factor, in particular of circular section, relative to the total weight of the paper.
- the dry weight amount of unsplit fibers of first form factor, based on the total weight of the paper, is preferably greater than or equal to 5%.
- the non-fibrillated synthetic fibers of first form factor have a number average length of between 3 and 6 mm, and a titer of between 0.3 and 1.7 dtex.
- the non-fibrillated synthetic fibers of first form factor have a titration of less than 2 dtex, better still less than 1 dtex, more preferably less than 0.5 dtex.
- the non-fibrillated synthetic fibers of first form factor are, for example, the fibers marketed under the reference mini Eslon by the company Woongjin, and are PET fibers of 0.3 dtex, or for example the fibers marketed under the reference EP023 by the Kuraray company, and are 0.33 dtex PET fibers.
- non-fibrillated synthetic fibers of first form factor in particular of circular section, may be polyvinylated 6.6 l, 7dTex 4mm fibers marketed by Rhodia or poly (ethylene terephthalate) fibers marketed by the company Kuraray under the reference EP023 5mm.
- the non-fibrillated synthetic fibers of first form factor may have the same color as the spun fibers or a different color.
- Non-fibrillated synthetic fibers of second form factor in particular of flat section, in particular rectangular
- These fibers are preferably fibers of "flattened" cross-section, that is to say synthetic fibers for which the section has a width greater than or equal to three times, preferably five times and more preferably 10 times, the thickness of this same section.
- the form factor of these fibers is preferably greater than or equal to 3, better still greater than or equal to 5, even more preferably greater than or equal to 10.
- the width of the section of the unshaped synthetic fibers with a second form factor section, in particular with a shape factor of at least 3, is preferably between 5 and 25 ⁇ , more preferably between 10 and 20 ⁇ .
- the thickness of the section of the unshaped synthetic fibers of second form factor, in particular of form factor greater than or equal to 3, is preferably between 0.5 and 10 ⁇ , more preferably between 1 and 5 ⁇ .
- the non-flashed synthetic fibers of second form factor are chosen from polyamide (PA), polyacrylic, polypropylene (PP) and poly (terephthalate) fibers.
- PET also referred to as polyester
- PVA polyvinyl alcohol
- aromatic polyester e.g., Vectran ® sold by Kuraray
- imide polyamide ethylene vinyl alcohol copolymer (EVOH) of polyolefin and preferably polyethylene (PE).
- PE polyethylene vinyl alcohol copolymer
- the non-flashed synthetic fibers of second form factor are more preferably polyamide and / or polyester fibers.
- non-flashed synthetic fibers of second form factor may be mixed polyester and polyamide fibers marketed by Kuraray, for example under the reference Wramp W101, or polyester fibers sold by the company Teijin, for example under the reference TA 14N.
- the paper according to the invention preferably comprises more than 10% by dry weight, better still more than 15% by dry weight and more preferably more than 25% by dry weight of unshaded synthetic fibers of second form factor, especially of factor of form greater than or equal to 3, relative to the total weight of the paper.
- the paper according to the invention preferably comprises less than 60% by dry weight, better less than 50% by dry weight and more preferably less than 40% by dry weight of non-fibrillated synthetic fibers of second form factor, in particular of factor of form greater than or equal to 3, relative to the total weight of the paper.
- the non-flashed synthetic fibers of second form factor especially of form factor greater than or equal to 3, have a length number average between 2 and 10 mm, preferably between 3 and 7 mm and more preferably between 5 and 6 mm, and a title between 0.2 and 3 dtex.
- the unshaped synthetic fibers of second form factor may have the same color as the unshaded fibers or a different color.
- the non-flashed synthetic fibers of second form factor are preferably obtained from multi-component ("splittable fiber") primary fibers, preferably two-component fibers.
- These primary fibers may be in the form of segmented ribbon, segmented cross, or may have a multilobal section, in particular trilobal, or a segmented circular section, hollow or not hollow Examples of such fibers are shown in Figures 1 to 6 described below.
- the two-component primary fibers 1 shown in these figures comprise a first component 2 and a second component 3. They are, for example, polyester and polyamide, respectively.
- FIG. 1 represents a two-component primary fiber 1 with a section segmented into sectors, called a "pie wedge fiber” ("pie wedge fiber").
- the sectors of one component alternate with those of the other component, around the axis of the fiber.
- the sectors separate in the pulp, during the manufacture of paper for example by stirring the fibrous suspension. In order to allow this separation (or cleavage), the sectors may be bonded together by a soluble glue.
- Such fibers are made by extrusion.
- FIG. 2 represents a two-component primary fiber 1 with a so-called “segmented ribbon fiber” section.
- FIG. 3 represents a two-component primary fiber 1 with a so-called “hollow pie wedge fiber” section.
- FIG. 4 represents a two-component primary fiber 1 with a so-called “segmented cross fiber” section.
- FIG. 5 represents a two-component primary fiber 1 with a so-called “tipped trilobal fiber” section.
- FIG. 6 represents a bicomponent primary fiber 1 with a multilayer section whose components alternate on one side of the section on the opposite side, called “conjugated"("conjugatedfiber” in English).
- the components of such primary fibers separate during their implementation for the manufacture of a paper according to the invention, so as to obtain said non-screened fibers with a second form factor section, in particular flattened with a factor of form greater than or equal to 3.
- the unsplit synthetic fibers with rectangular section are preferably obtained from two-component cross-section fibers.
- the non-flashed synthetic fibers of second form factor have a titration of less than 3 dtex.
- the non-flashed synthetic fibers of second form factor, in particular of form factor greater than or equal to 3, are for example the fibers sold under the reference TA 14N by the company Teijin, and are polyester fibers, or come for example dissociation of the fibers sold under the name Wramp W101 by Kuraray, which are polyester / polyamide conjugated two-component fibers of 3.3 dtex before cleavage.
- the multicomponent primary fibers when they are dissociated, can produce only unsplit synthetic fibers with form factors of greater than or equal to 3. As a variant, they produce at the same time fibers with a shape factor of strictly less than 3, in particular 2, better at 1.1, and fibers of form factor strictly greater than 3. All of the unshaped synthetic fibers of the invention, whose shape factors are different, can come from the dissociation of the same type of primary fibers. In a variant, the mixture of unsplit synthetic fibers of different form factors, according to the invention, comes both from the introduction of fibers having a first form factor, in particular of circular section fibers, and multicomponent primary fibers. , in particular two-component.
- the paper according to the invention may comprise less than 5% by dry weight of non-synthetic fibers, such as cellulosic fibers, relative to the total weight of the paper, and preferably less than 2% by dry weight of non-cellulosic fibers by report to the total weight of the paper, still better be free of non-synthetic fibers, such as cellulosic fibers.
- the fibers of the paper according to the invention consist exclusively of synthetic fibers and non-glossy synthetic fibers.
- a polymeric binder such as polyvinyl alcohol (PVA) or a styrene-acrylic copolymer, which has a synergy with the synthetic fibers.
- PVA polyvinyl alcohol
- styrene-acrylic copolymer which has a synergy with the synthetic fibers.
- the application of the polymeric binder may be by impregnation, surfacing or coating, preferably the polymeric binder being introduced at least partially by mass.
- the composition may comprise an anionic polymeric dispersion, in particular flocculated.
- the composition comprises at least 3% by dry weight of anionic polymeric dispersion, in particular flocculated.
- anionic polymeric dispersion improves the wet tensile strength, the cohesion and the folding resistance of the paper.
- the latex used is, for example, the latex marketed by Dow Chemicals under the reference 94755.04 or a latex as described in the international application WO2008152299 or the application WO2014083527.
- the formulation of the paper according to the invention may also comprise a main cationic flocculating agent, in an amount of between 1 and 5% by dry weight relative to the total weight of the paper, and optionally a secondary cationic flocculating agent, in an amount between 0.1 and 0.5% by dry weight, chosen from a cationic resin, polyacrylamides, polyethyleneimines, polyvinylamines and their mixtures, preferably a cationic resin, and better a polyamide-amine-epichloridin resin.
- a main cationic flocculating agent in an amount of between 1 and 5% by dry weight relative to the total weight of the paper
- a secondary cationic flocculating agent in an amount between 0.1 and 0.5% by dry weight, chosen from a cationic resin, polyacrylamides, polyethyleneimines, polyvinylamines and their mixtures, preferably a cationic resin, and better a polyamide-amine-epichloridin resin.
- binders may be used, including a transparent or translucent elastomeric binder, such as a polyurethane and a colloidal silica, or an acrylic polymer binder or styrene-acrylic copolymer.
- a transparent or translucent elastomeric binder such as a polyurethane and a colloidal silica
- an acrylic polymer binder or styrene-acrylic copolymer may be incorporated into the paper by anionic dispersion, especially in a proportion of between 5 and 45.degree. % by dry weight relative to the total weight of the paper.
- the paper according to the invention may comprise any adjuvants and compounds conventionally used in the manufacture of papermaking paper, such as fillers, retention agents, bonding agents and / or resistance agents in the state. wet, especially epichlorohydrin resins.
- the paper according to the invention can in particular comprise filler-blocking filler, in particular plastic filler such as, for example, polyvinyl chloride (PVC) particles marketed by Kern One under the reference Lacovyl Pb 1302.
- plastic filler such as, for example, polyvinyl chloride (PVC) particles marketed by Kern One under the reference Lacovyl Pb 1302.
- PVC polyvinyl chloride
- the paper according to the invention can be manufactured according to the usual manufacturing techniques of cellulosic papers, except the steps specifically related to the presence of cellulosic fibers if they are absent.
- the refining step which is particularly energy-consuming, can be advantageously suppressed.
- the manufacturing method can be adapted to the presence of security elements such as a watermark or security thread.
- the paper preferably has a hand less than or equal to 2.5 cm 3 / g, better a hand less than or equal to 2 cm 3 / g and more preferably less than or equal to 1.5 cm 3 / g.
- the paper may have a thickness between 100 and 300 ⁇ , better between 100 and 150 ⁇ . It is measured according to ISO 534 "Paper and board - Determination of thickness, density and specific volume”.
- the basis weight of the paper may be between 70 g / m 2 and 150 g / m 2 and preferably between 90 g / m 2 and 110 g / m 2 . It is measured according to ISO 536 "Paper and board - Determination of grammage”. Watermark
- the paper according to the invention may comprise a watermark.
- This watermark can be formed on round shape or flat table.
- the watermark may be of any known type, for example clear and / or dark, possibly multiton or multi-toned, for example as described in patent EP 1 122 360, EP 2 350 384 and EP 2 550 395.
- the paper according to the invention may comprise a security thread introduced in bulk or between two jets of paper according to the invention bonded in the wet phase.
- the security thread can be at least partially introduced into the paper.
- the paper may comprise a fibrous ribbon, in particular a cellulosic fibrous ribbon as described in the application WO2008043965, a plastic ribbon or a knitted ribbon, especially as described in the application WO2006016088.
- the wire may be metallized and / or holographic and / or interferential and / or provided with optical structures, including lenses or mirrors.
- the paper according to the invention can be single or multijet.
- the jets may or may not have the same fibrous composition.
- the paper may comprise firstly a jet of synthetic fibers according to the invention, and secondly a jet of cellulosic fibers, assembled in wet phase, the jet according to the invention then constituting a reinforcing jet.
- the paper may comprise, on the one hand, a jet of synthetic fibers, especially of the invention, whose fibrous composition promotes the formation of the sheet, especially the epair, and the rendering of the watermark, and other a synthetic fiber jet according to the invention whose fibrous composition promotes the mechanical strength properties, said jets being assembled in the wet phase.
- the jets can be of the same color or not.
- the Bendsten porosity of the paper may be between 0 mL / min and 10,000 mL / min, better still between 1 mL / min and 7000 mL / min. It is measured according to ISO 5636-3 "Paper and cardboard; determination of air permeability (average value); Part 3: Bendtsen method »
- the double fold folding resistance Schopper of the paper according to the invention is greater than 5000, more preferably greater than 20000, more preferably greater than 50000. It is measured according to ISO 5626 "Paper; determination of the folding resistance ".
- the tear strength of the paper (measured according to the standard
- ISO 1974 is greater than 1000 mN, more preferably greater than 2000 mN, more preferably greater than 3000 mN. It is measured according to ISO 1974 "Paper - Determination of tear strength - Elmendorf method"
- the invention makes it possible to obtain a synthetic paper whose mechanical properties, in particular the resistance to bending and tearing, are superior to those of a conventional paper, while at the same time allowing, if it is desired, to produce watermarks of quality and quality. satisfactory resolution.
- the paper according to the invention preferably comprises a security element, in particular a watermark or a security thread, for example a thread introduced into window (s), as mentioned above.
- the invention also relates to a secure document comprising a paper according to the invention.
- the secure document is a bank note.
- the secure document can also be another type of payment method such as a check or a restaurant ticket, an identity document such as an identity card, a visa, a passport, including the personal data page of a passport, a secure label, a heat-shrinkable secure sleeve, a "prelam” or "inlay” insert for a passport or card, in particular a smart card, or a driver's license, a lottery ticket, a ticket, a ticket entrance to cultural or sports events, a playing card or a card to collect.
- An insert is a layer supporting a contactless communication device, preferably radio frequency.
- the paper according to the invention and / or the secure document made with the paper according to the invention may comprise one or more additional security elements as defined below.
- security elements comprise for example colored fibers or boards. These security elements are called first level.
- Additional security elements are detectable only with a relatively simple apparatus, such as a lamp emitting in the ultraviolet (UV) or infrared (IR).
- UV ultraviolet
- IR infrared
- These security elements comprise for example fibers, boards or particles. These security elements may be visible to the naked eye or not, being for example luminescent under a lighting of a Wood lamp emitting in a wavelength of 365 nm. These security elements are said to be second level.
- Additional security elements require for their detection a more sophisticated detection device.
- These security elements are for example capable of generating a specific signal when they are subjected, simultaneously or not, to one or more external excitation sources. The automatic detection of the signal makes it possible to authenticate, if necessary, the document.
- These security elements comprise, for example, tracers in the form of active materials, particles or fibers capable of generating a specific signal when these tracers are subjected to optronic, electrical, magnetic or electromagnetic excitation. These security elements are said to be third level.
- the additional security element (s) present in the paper according to the invention or the secure document according to the invention may have first, second or third level security features.
- the additional safety element or elements can be fixed to the document by simple heating, thus avoiding the use of a hot-activatable adhesive. Comparative tests
- the tear resistance is measured according to the ISO 1974 standard.
- the thickness is measured according to the ISO 534 standard and makes it possible to obtain the hand (or mass volume) which is equal to the thickness divided by the grammage,
- the quality of the watermark is assessed visually by a score ranging from 1 (bad) to 6 (very good).
- the raw substrates that is to say without any treatment as defined above, and the substrates surfaced, that is to say, impregnated with a polyvinyl alcohol composition or a composition of styrene-acrylic copolymer are tested.
- Example 2 The properties of a substrate whose fibrous composition is composed only of synthetic fibers and non-glossy synthetic fibers circular section (Example 1) were compared to those of a substrate whose fibrous composition corresponds to that of the Example 1 except that a portion of the unshaped synthetic fibers of circular section is replaced by unsplit synthetic fibers of rectangular section (Example 2).
- Example 1 The results, shown in the table below, reflect the fact that the mixture of unshaped synthetic fibers of different sections and of different form factors, in this case circular and rectangular sections, makes it possible to increase the resistance to tearing and folding resistance without unduly degrading the quality of the watermark. Satisfactory properties are then obtained, in particular good tear strength.
- Example 2 The results, shown in the table below, reflect the fact that the mixture of unshaped synthetic fibers of different sections and of different form factors, in this case circular and rectangular sections, makes it possible to increase the resistance to tearing and folding resistance without unduly degrading the quality of the watermark. Satisfactory properties are then obtained, in particular good tear strength.
- Example 2 Example 2
- the proportions are mass.
- Example 3 The properties of a substrate whose fibrous composition is composed of glossy synthetic fibers and of unsplit synthetic fibers with a circular section (Example 3) were compared with those of a substrate whose fibrous composition corresponds to that of the example 3 apart from the fact that the unsecured synthetic fibers with circular section are completely replaced by unsplit synthetic fibers of rectangular section (Example 4).
- the proportions are mass.
- the proportions are mass.
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Paper (AREA)
Abstract
Description
Claims
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
FR1552397A FR3034110B1 (en) | 2015-03-23 | 2015-03-23 | PAPER COMPRISING SYNTHETIC FIBERS |
PCT/EP2016/056355 WO2016151004A1 (en) | 2015-03-23 | 2016-03-23 | Paper containing synthetic fibres |
Publications (2)
Publication Number | Publication Date |
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EP3274502A1 true EP3274502A1 (en) | 2018-01-31 |
EP3274502B1 EP3274502B1 (en) | 2021-08-04 |
Family
ID=53177657
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP16711006.3A Active EP3274502B1 (en) | 2015-03-23 | 2016-03-23 | Paper containing synthetic fibres |
Country Status (8)
Country | Link |
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EP (1) | EP3274502B1 (en) |
KR (1) | KR20170140209A (en) |
CN (1) | CN107667198B (en) |
BR (1) | BR112017020295A2 (en) |
FR (1) | FR3034110B1 (en) |
PH (1) | PH12017501734A1 (en) |
RU (1) | RU2698693C2 (en) |
WO (1) | WO2016151004A1 (en) |
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US2810646A (en) * | 1953-09-17 | 1957-10-22 | American Cyanamid Co | Water-laid webs comprising water-fibrillated, wet-spun filaments of an acrylonitrile polymer and method of producing them |
FR1317778A (en) | 1961-03-16 | 1963-05-08 | ||
GB1401599A (en) | 1971-10-29 | 1975-07-16 | Gulf Research Development Co | Fibril and process |
US4247318A (en) | 1979-01-30 | 1981-01-27 | E. I. Du Pont De Nemours And Company | Process for making security paper from film-fibril sheets |
IN157644B (en) | 1981-02-19 | 1986-05-10 | Portals Ltd | |
NZ201691A (en) | 1981-08-24 | 1985-08-30 | Commw Scient Ind Res Org | Security token made from bi-axially oriented polymeric film |
US5449200A (en) | 1993-06-08 | 1995-09-12 | Domtar, Inc. | Security paper with color mark |
US5954920A (en) * | 1994-06-07 | 1999-09-21 | Kuraray Co., Ltd. | Paper comprising aromatic polyester and process for producing the same |
US5698333A (en) | 1994-06-27 | 1997-12-16 | Mobil Oil Corporation | Multilayer film structures for use in the production of banknotes or the like |
GB2338680B (en) | 1998-06-25 | 2000-05-17 | Rue De Int Ltd | Improvementd in security documents and subtrates therefor |
FR2804447B1 (en) | 2000-02-01 | 2002-04-05 | Arjo Wiggins Sa | PAPER COMPRISING A MULTI-TONING FILIGRANE AND CANVAS FOR MANUFACTURING THIS PAPER |
FR2816643B1 (en) | 2000-11-13 | 2003-01-03 | Arjo Wiggins Sa | PRINTABLE COMPLEX SECURITY MEDIUM AND MANUFACTURING METHOD THEREOF |
GB2381539B (en) | 2001-11-05 | 2003-11-05 | Rue De Int Ltd | Paper incorporating a wide elongate impermeable element, and a method of makingof the same |
DE10163381A1 (en) | 2001-12-21 | 2003-07-03 | Giesecke & Devrient Gmbh | Security paper and method and device for its production |
GB2388377B (en) | 2002-05-09 | 2004-07-28 | Rue De Int Ltd | A paper sheet incorporating a security element and a method of making the same |
DE10243653A1 (en) | 2002-09-19 | 2004-04-01 | Giesecke & Devrient Gmbh | security paper |
FR2873134B1 (en) | 2004-07-15 | 2011-07-15 | Arjowiggins | KNITTED STRUCTURE INTENDED TO BE INCORPORATED IN SHEET MATERIAL AND SHEET MATERIAL INCORPORATING SUCH A STRUCTURE |
ATE454980T1 (en) | 2004-12-23 | 2010-01-15 | Landqart | MULTI-LAYER STRUCTURE AS A PRINTING SUBSTRATE AND METHOD FOR THE PRODUCTION THEREOF |
US7462392B2 (en) * | 2006-02-03 | 2008-12-09 | W. R. Grace & Co.-Conn. | Bi-tapered reinforcing fibers |
DE102006022703A1 (en) | 2006-05-12 | 2007-11-15 | Giesecke & Devrient Gmbh | bill |
FR2907136B1 (en) | 2006-10-12 | 2010-01-15 | Arjowiggins | SECURITY TAPE, SHEET AND SECURITY DOCUMENT COMPRISING IT AND METHOD OF INCORPORATING IT |
FR2916768B1 (en) * | 2007-05-31 | 2009-07-24 | Arjowiggins Licensing Soc Par | CRISIS RESISTANT SECURITY SHEET, METHOD FOR MANUFACTURING SAME, AND SAFETY DOCUMENT COMPRISING SAME |
FR2925864B1 (en) | 2007-12-28 | 2012-08-31 | Arjowiggins Licensing Sas | SAFETY SHEET COMPRISING A COEXTRUDE SUPPORT |
CA2737578A1 (en) | 2008-09-26 | 2010-04-01 | Vhp Veiligheidspapierfabriek Ugchelen B.V. | Method for producing a watermark element, watermark element, and also applications |
JP2012529155A (en) | 2009-06-04 | 2012-11-15 | ライドール,インコーポレーテッド | Electrical insulating materials and their manufacture and use |
FR2957943B1 (en) | 2010-03-24 | 2021-11-05 | Arjowiggins Security | WATERMARK, METHODS FOR MANUFACTURING A PART FOR THE FORMATION OF A WATERMARK AND PART OBTAINED ACCORDING TO THIS PROCEDURE |
US9353480B2 (en) * | 2012-04-11 | 2016-05-31 | Ahlstrom Corporation | Sterilizable and printable nonwoven packaging materials |
FR2998588B1 (en) | 2012-11-29 | 2015-01-30 | Arjowiggins Security | FACTOR RESISTANT SAFETY SHEET, PROCESS FOR PRODUCING THE SAME, AND SAFETY DOCUMENT COMPRISING THE SAME. |
US9617685B2 (en) * | 2013-04-19 | 2017-04-11 | Eastman Chemical Company | Process for making paper and nonwoven articles comprising synthetic microfiber binders |
-
2015
- 2015-03-23 FR FR1552397A patent/FR3034110B1/en not_active Expired - Fee Related
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2016
- 2016-03-23 KR KR1020177030499A patent/KR20170140209A/en not_active Application Discontinuation
- 2016-03-23 BR BR112017020295-6A patent/BR112017020295A2/en active Search and Examination
- 2016-03-23 WO PCT/EP2016/056355 patent/WO2016151004A1/en active Application Filing
- 2016-03-23 EP EP16711006.3A patent/EP3274502B1/en active Active
- 2016-03-23 RU RU2017133219A patent/RU2698693C2/en active
- 2016-03-23 CN CN201680029472.7A patent/CN107667198B/en not_active Expired - Fee Related
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2017
- 2017-09-20 PH PH12017501734A patent/PH12017501734A1/en unknown
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RU2017133219A (en) | 2019-04-23 |
KR20170140209A (en) | 2017-12-20 |
EP3274502B1 (en) | 2021-08-04 |
PH12017501734A1 (en) | 2018-03-12 |
RU2017133219A3 (en) | 2019-04-23 |
WO2016151004A1 (en) | 2016-09-29 |
RU2698693C2 (en) | 2019-08-28 |
FR3034110A1 (en) | 2016-09-30 |
CN107667198B (en) | 2020-04-03 |
CN107667198A (en) | 2018-02-06 |
FR3034110B1 (en) | 2017-04-21 |
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