Classifications

• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B32—LAYERED PRODUCTS
  • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
  • B32B38/00—Ancillary operations in connection with laminating processes
  • B32B38/08—Impregnating
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
  • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
  • B29C53/00—Shaping by bending, folding, twisting, straightening or flattening; Apparatus therefor
  • B29C53/56—Winding and joining, e.g. winding spirally
  • B29C53/58—Winding and joining, e.g. winding spirally helically
  • B29C53/60—Winding and joining, e.g. winding spirally helically using internal forming surfaces, e.g. mandrels
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B32—LAYERED PRODUCTS
  • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
  • B32B1/00—Layered products having a non-planar shape
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B32—LAYERED PRODUCTS
  • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
  • B32B27/00—Layered products comprising a layer of synthetic resin
  • B32B27/06—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material
  • B32B27/08—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B32—LAYERED PRODUCTS
  • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
  • B32B27/00—Layered products comprising a layer of synthetic resin
  • B32B27/12—Layered products comprising a layer of synthetic resin next to a fibrous or filamentary layer
• • B—PERFORMING OPERATIONS; TRANSPORTING
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  • B32B27/00—Layered products comprising a layer of synthetic resin
  • B32B27/18—Layered products comprising a layer of synthetic resin characterised by the use of special additives
  • B32B27/22—Layered products comprising a layer of synthetic resin characterised by the use of special additives using plasticisers
• • B—PERFORMING OPERATIONS; TRANSPORTING
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  • B32B27/00—Layered products comprising a layer of synthetic resin
  • B32B27/30—Layered products comprising a layer of synthetic resin comprising vinyl (co)polymers; comprising acrylic (co)polymers
  • B32B27/304—Layered products comprising a layer of synthetic resin comprising vinyl (co)polymers; comprising acrylic (co)polymers comprising vinyl halide (co)polymers, e.g. PVC, PVDC, PVF, PVDF
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B32—LAYERED PRODUCTS
  • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
  • B32B27/00—Layered products comprising a layer of synthetic resin
  • B32B27/30—Layered products comprising a layer of synthetic resin comprising vinyl (co)polymers; comprising acrylic (co)polymers
  • B32B27/306—Layered products comprising a layer of synthetic resin comprising vinyl (co)polymers; comprising acrylic (co)polymers comprising vinyl acetate or vinyl alcohol (co)polymers
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B32—LAYERED PRODUCTS
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  • B32B27/00—Layered products comprising a layer of synthetic resin
  • B32B27/34—Layered products comprising a layer of synthetic resin comprising polyamides
• • B—PERFORMING OPERATIONS; TRANSPORTING
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  • B32B27/00—Layered products comprising a layer of synthetic resin
  • B32B27/38—Layered products comprising a layer of synthetic resin comprising epoxy resins
• • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
  • F17—STORING OR DISTRIBUTING GASES OR LIQUIDS
  • F17C—VESSELS FOR CONTAINING OR STORING COMPRESSED, LIQUEFIED OR SOLIDIFIED GASES; FIXED-CAPACITY GAS-HOLDERS; FILLING VESSELS WITH, OR DISCHARGING FROM VESSELS, COMPRESSED, LIQUEFIED, OR SOLIDIFIED GASES
  • F17C1/00—Pressure vessels, e.g. gas cylinder, gas tank, replaceable cartridge
  • F17C1/02—Pressure vessels, e.g. gas cylinder, gas tank, replaceable cartridge involving reinforcing arrangements
• • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
  • F17—STORING OR DISTRIBUTING GASES OR LIQUIDS
  • F17C—VESSELS FOR CONTAINING OR STORING COMPRESSED, LIQUEFIED OR SOLIDIFIED GASES; FIXED-CAPACITY GAS-HOLDERS; FILLING VESSELS WITH, OR DISCHARGING FROM VESSELS, COMPRESSED, LIQUEFIED, OR SOLIDIFIED GASES
  • F17C1/00—Pressure vessels, e.g. gas cylinder, gas tank, replaceable cartridge
  • F17C1/16—Pressure vessels, e.g. gas cylinder, gas tank, replaceable cartridge constructed of plastics materials
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
  • B29L—INDEXING SCHEME ASSOCIATED WITH SUBCLASS B29C, RELATING TO PARTICULAR ARTICLES
  • B29L2031/00—Other particular articles
  • B29L2031/712—Containers; Packaging elements or accessories, Packages
  • B29L2031/7154—Barrels, drums, tuns, vats
  • B29L2031/7156—Pressure vessels
• • B—PERFORMING OPERATIONS; TRANSPORTING
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• • B—PERFORMING OPERATIONS; TRANSPORTING
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• • B—PERFORMING OPERATIONS; TRANSPORTING
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  • B32B2260/00—Layered product comprising an impregnated, embedded, or bonded layer wherein the layer comprises an impregnation, embedding, or binder material
  • B32B2260/02—Composition of the impregnated, bonded or embedded layer
  • B32B2260/021—Fibrous or filamentary layer
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B32—LAYERED PRODUCTS
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  • B32B2260/00—Layered product comprising an impregnated, embedded, or bonded layer wherein the layer comprises an impregnation, embedding, or binder material
  • B32B2260/04—Impregnation, embedding, or binder material
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• • B—PERFORMING OPERATIONS; TRANSPORTING
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  • B32B2262/00—Composition or structural features of fibres which form a fibrous or filamentary layer or are present as additives
  • B32B2262/10—Inorganic fibres
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• • B—PERFORMING OPERATIONS; TRANSPORTING
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  • B32B2262/00—Composition or structural features of fibres which form a fibrous or filamentary layer or are present as additives
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• • B—PERFORMING OPERATIONS; TRANSPORTING
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• • B—PERFORMING OPERATIONS; TRANSPORTING
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• • B—PERFORMING OPERATIONS; TRANSPORTING
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  • B32B2307/00—Properties of the layers or laminate
  • B32B2307/70—Other properties
  • B32B2307/724—Permeability to gases, adsorption
  • B32B2307/7242—Non-permeable
• • B—PERFORMING OPERATIONS; TRANSPORTING
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• • B—PERFORMING OPERATIONS; TRANSPORTING
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  • B32B2377/00—Polyamides
• • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
  • F17—STORING OR DISTRIBUTING GASES OR LIQUIDS
  • F17C—VESSELS FOR CONTAINING OR STORING COMPRESSED, LIQUEFIED OR SOLIDIFIED GASES; FIXED-CAPACITY GAS-HOLDERS; FILLING VESSELS WITH, OR DISCHARGING FROM VESSELS, COMPRESSED, LIQUEFIED, OR SOLIDIFIED GASES
  • F17C2203/00—Vessel construction, in particular walls or details thereof
  • F17C2203/06—Materials for walls or layers thereof; Properties or structures of walls or their materials
  • F17C2203/0602—Wall structures; Special features thereof
  • F17C2203/0604—Liners
• • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
  • F17—STORING OR DISTRIBUTING GASES OR LIQUIDS
  • F17C—VESSELS FOR CONTAINING OR STORING COMPRESSED, LIQUEFIED OR SOLIDIFIED GASES; FIXED-CAPACITY GAS-HOLDERS; FILLING VESSELS WITH, OR DISCHARGING FROM VESSELS, COMPRESSED, LIQUEFIED, OR SOLIDIFIED GASES
  • F17C2203/00—Vessel construction, in particular walls or details thereof
  • F17C2203/06—Materials for walls or layers thereof; Properties or structures of walls or their materials
  • F17C2203/0602—Wall structures; Special features thereof
  • F17C2203/0609—Straps, bands or ribbons
• • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
  • F17—STORING OR DISTRIBUTING GASES OR LIQUIDS
  • F17C—VESSELS FOR CONTAINING OR STORING COMPRESSED, LIQUEFIED OR SOLIDIFIED GASES; FIXED-CAPACITY GAS-HOLDERS; FILLING VESSELS WITH, OR DISCHARGING FROM VESSELS, COMPRESSED, LIQUEFIED, OR SOLIDIFIED GASES
  • F17C2203/00—Vessel construction, in particular walls or details thereof
  • F17C2203/06—Materials for walls or layers thereof; Properties or structures of walls or their materials
  • F17C2203/0602—Wall structures; Special features thereof
  • F17C2203/0612—Wall structures
  • F17C2203/0614—Single wall
  • F17C2203/0619—Single wall with two layers
• • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
  • F17—STORING OR DISTRIBUTING GASES OR LIQUIDS
  • F17C—VESSELS FOR CONTAINING OR STORING COMPRESSED, LIQUEFIED OR SOLIDIFIED GASES; FIXED-CAPACITY GAS-HOLDERS; FILLING VESSELS WITH, OR DISCHARGING FROM VESSELS, COMPRESSED, LIQUEFIED, OR SOLIDIFIED GASES
  • F17C2203/00—Vessel construction, in particular walls or details thereof
  • F17C2203/06—Materials for walls or layers thereof; Properties or structures of walls or their materials
  • F17C2203/0634—Materials for walls or layers thereof
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  • F17C2203/066—Plastics
• • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
  • F17—STORING OR DISTRIBUTING GASES OR LIQUIDS
  • F17C—VESSELS FOR CONTAINING OR STORING COMPRESSED, LIQUEFIED OR SOLIDIFIED GASES; FIXED-CAPACITY GAS-HOLDERS; FILLING VESSELS WITH, OR DISCHARGING FROM VESSELS, COMPRESSED, LIQUEFIED, OR SOLIDIFIED GASES
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• • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
  • F17—STORING OR DISTRIBUTING GASES OR LIQUIDS
  • F17C—VESSELS FOR CONTAINING OR STORING COMPRESSED, LIQUEFIED OR SOLIDIFIED GASES; FIXED-CAPACITY GAS-HOLDERS; FILLING VESSELS WITH, OR DISCHARGING FROM VESSELS, COMPRESSED, LIQUEFIED, OR SOLIDIFIED GASES
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• • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
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• • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
  • F17—STORING OR DISTRIBUTING GASES OR LIQUIDS
  • F17C—VESSELS FOR CONTAINING OR STORING COMPRESSED, LIQUEFIED OR SOLIDIFIED GASES; FIXED-CAPACITY GAS-HOLDERS; FILLING VESSELS WITH, OR DISCHARGING FROM VESSELS, COMPRESSED, LIQUEFIED, OR SOLIDIFIED GASES
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• • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
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• • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
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• • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
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  • F17C2221/00—Handled fluid, in particular type of fluid
  • F17C2221/01—Pure fluids
  • F17C2221/012—Hydrogen
• • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
  • F17—STORING OR DISTRIBUTING GASES OR LIQUIDS
  • F17C—VESSELS FOR CONTAINING OR STORING COMPRESSED, LIQUEFIED OR SOLIDIFIED GASES; FIXED-CAPACITY GAS-HOLDERS; FILLING VESSELS WITH, OR DISCHARGING FROM VESSELS, COMPRESSED, LIQUEFIED, OR SOLIDIFIED GASES
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• • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
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• • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
  • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
  • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
  • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
  • Y02E60/30—Hydrogen technology
  • Y02E60/32—Hydrogen storage
• • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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  • Y02P90/00—Enabling technologies with a potential contribution to greenhouse gas [GHG] emissions mitigation
  • Y02P90/45—Hydrogen technologies in production processes

Definitions

• TITLE MULTI-LAYER STRUCTURE FOR THE TRANSPORT OR STORAGE OF
• the present patent application relates to composite multilayer structures for the transport, distribution or storage of hydrogen, in particular for the distribution or storage of hydrogen, and their manufacturing process.
• Hydrogen tanks are a subject that is currently attracting a lot of interest from many manufacturers, especially in the automotive field.
• One of the goals is to offer vehicles that pollute less and less.
• electric or hybrid vehicles comprising a battery aim to gradually replace thermal vehicles, such as gasoline or diesel vehicles.
• thermal vehicles such as gasoline or diesel vehicles.
• the battery is a relatively complex component of the vehicle.
• the electric vehicle still suffers today from several problems, namely the autonomy of the battery, the use in these rare earth batteries whose resources are not inexhaustible, recharging times much longer than the durations. tank filling, as well as a problem of electricity production in the different countries to be able to recharge the batteries.
• Hydrogen therefore represents an alternative to the electric battery since hydrogen can be transformed into electricity by means of a fuel cell and thus power electric vehicles.
• Hydrogen tanks generally consist of a metal casing (liner or sealing layer) which must prevent the permeation of hydrogen.
• liner or sealing layer One of the types of tanks being considered, called Type IV, is based on a thermoplastic liner around which a composite is wrapped.
• thermoplastic resin liner or sealing sheath
• a reinforcing structure made up of fibers (glass, aramid, carbon). called sheath or reinforcing layer which allow to work at much higher pressures while reducing the mass and avoiding the risk of explosive rupture in the event of severe external attacks.
• the permeability of the liner is indeed a key factor in limiting hydrogen losses from the tank;
• the first generation of type IV tanks used a liner based on high density polyethylene (HDPE).
• HDPE high density polyethylene
• HDPE has the drawback of having too low a melting temperature and high hydrogen permeability, which is a problem with the new thermal withstand requirements and does not allow the filling speed of the tank to be increased. tank.
• PA6 polyamide
• Application US2014 / 008373 describes a lightweight storage cylinder for a high pressure compressed gas, the cylinder having a liner wrapped in a stress layer, the liner comprising: a first inner layer of impact modified polyamide (PA) in contact with gas, an outer thermoplastic layer in contact with the stress layer; and an adhesive tie layer between the first impact modified inner PA layer and the outer thermoplastic layer.
• PA impact modified polyamide
• French application FR2923575 describes a reservoir for storing fluid under high pressure comprising at each of its ends along its axis a nozzle metal end, a liner enveloping said end caps and a structural layer of fiber impregnated with thermosetting resin enveloping said liner.
• WO1 8155491 describes a hydrogen transport component having a three-layer structure, the inner layer of which is a composition consisting of PA11, 15 to 50% of an impact modifier and 1 to 3% of plasticizer or without plasticizer which exhibits hydrogen barrier properties, good flexibility and durability at low temperature.
• this structure is suitable for pipes for transporting hydrogen but not for storing hydrogen.
• the matrix of the composite in order to optimize its mechanical resistance at high temperature and on the other hand the material composing the sealing sheath, in order to optimize its processing temperature.
• the possible modification of the composition of the material composing the sealing sheath, which will be made, must not result in a significant increase in the manufacturing temperature (extrusion-blow molding, injection, rotomoulding, etc.) of this liner, compared to what is practiced today.
• the present invention therefore relates to a multilayer structure intended for the transport, distribution and storage of hydrogen, in particular for the storage of hydrogen, comprising from the inside to the outside a sealing layer (1) and at least one composite reinforcing layer (2), said waterproofing layer comprising from the inside to the outside: a layer (a) consisting of a composition mainly comprising: a thermoplastic polyamide polymer with a short chain and whose Tf , as measured according to ISO 11357-3: 2013, is greater than 160 ° C, in particular greater than 170 ° C, more than 15% and up to 50% of impact modifier, or comprising mainly: a thermoplastic polyamide polymer with long semi-crystalline chain and whose Tm, as measured according to ISO 11357-3: 2013, is greater than 160 ° C, in particular greater than 170 ° C, up to 50% by weight of impact modifier, in particular up to less than 15% by weight of impact modifier, in particular up to 12% by weight of impact modifier relative to the total weight of the composition, up to 3% by weight of plasticizer relative to
• PVDF corresponds to polyvinylidene fluoride.
• EVOH stands for ethylene vinyl alcohol.
• the Tm of the short-chain polyamide thermoplastic polymer is greater than 200 ° C.
• thermoplastic polyamide polymer with a short semi-crystalline chain strongly impact modified or long semi-crystalline chain and comprising a proportion of impact modifier and plasticizer limited above and above.
• a barrier layer for the waterproofing layer, with a different polymer for the matrix of the composite and in particular an epoxy resin or epoxy-based, said composite being wound on the waterproofing layer, made it possible to obtain a structure suitable for transporting, distributing or storing hydrogen and in particular an increase in the maximum temperature of use which can go up to 120 ° C, thus making it possible to increase the filling speed of the tanks.
• multilayer structure should be understood to mean a reservoir comprising or made up of several layers, namely a sealing layer comprising at least three layers and at least one reinforcing layer, in particular a single reinforcing layer.
• the multilayer structure is therefore meant to the exclusion of a pipe or tube.
• the tank can be a tank for the mobile storage of hydrogen, i.e. on a truck for the transport of hydrogen, on a car for the transport of hydrogen and the supply of hydrogen d '' a fuel cell for example, on a train for the supply of hydrogen or on a drone for the supply of hydrogen, but it can also be a stationary storage tank for hydrogen in a station for the distribution of hydrogen to vehicles.
• said short-chain or long-chain thermoplastic polyamide polymer of layer (a) is to the exclusion of a polyether block amide (PEBA).
• PEBA polyether block amide
• Poly ether block amide are copolymers with amide units (Ba1) and polyether units (Ba2), said amide unit (Ba1) corresponding to an aliphatic repeating unit chosen from a unit obtained from at least one amino acid or a unit obtained from at least one lactam, or an XY unit obtained from polycondensation:
• diamine being preferably chosen from a linear or branched aliphatic diamine or a mixture thereof, and
• dicarboxylic acid being preferably chosen from: a linear or branched aliphatic dicacid, or a mixture of these, said diamine and said dicacid comprising from 4 to 36 carbon atoms, advantageously from 6 to 18 carbon atoms; said polyether units (Ba2) being in particular derived from at least one polyalkylene ether polyol, in particular a polyalkylene ether diol.
• composition of layer (a) is devoid of nucleating agent.
• Nucleating agents are known to those skilled in the art and refer to a substance which, when incorporated into a polymer, forms nuclei for crystal growth in the molten polymer.
• They can be chosen, for example, from micro talc, carbon black, silica, titanium dioxide and nanoclays.
• said short-chain or long-chain thermoplastic polyamide polymer of layer (a) is to the exclusion of a polyether block amide (PEBA) and said composition of layer (a) is devoid of agent. nucleating.
• PEBA polyether block amide
• said short-chain or long-chain polyamide thermoplastic polymer of layer (b) is to the exclusion of a polyether block amide (PEBA).
• said composition of layer (b) is devoid of nucleating agent
• said short-chain or long-chain thermoplastic polyamide polymer of layer (b) is excluding a polyether block amide (PEBA) and said composition of layer (b) is devoid of agent. nucleating.
• PEBA polyether block amide
• said short-chain or long-chain thermoplastic polyamide polymer of layer (a) and of layer (b) is to the exclusion of a polyether block amide (PEBA).
• PEBA polyether block amide
• said composition of layer (a) and of layer (b) is devoid of nucleating agent.
• said short-chain or long-chain thermoplastic polyamide polymer of layer (a) and of layer (b) is excluding a polyether block amide (PEBA) and said composition of the layer ( a) and layer (b) is devoid of nucleating agent.
• PEBA polyether block amide
• said multilayer structure consists of a waterproofing layer and a reinforcing layer.
• the sealing layer (1) is impermeable to hydrogen at 23 ° C, that is to say that the permeability to hydrogen at 23 ° C is less than 500 cc.mm/m2. 24h. .atm at 23 ° C under 0% relative humidity (RH).
• PA11 is excluded from the composition of layer (a).
• PA11 is excluded from the composition of layer (b).
• PA11 is excluded from the composition of layer (a) and from the composition of layer (b).
• the composite reinforcing layer (s) is (are) wound (s) around the waterproofing layer by means of tapes (or tapes or rovings) of fibers impregnated with polymer which are deposited, for example, by filament winding.
• the polymers are different.
• the polymers of the reinforcing layers are identical, there may be several layers present, but advantageously, only one reinforcing layer is present and which then has at least one complete winding around the waterproofing layer.
• the outermost layer (b) of said sealing layer may or may not adhere to the outermost layer. internal of said composite reinforcement.
• the other composite reinforcement layers may or may not also adhere to each other.
• the other waterproofing layers may or may not adhere to each other.
• only a waterproofing layer and a reinforcing layer are present and do not adhere to each other.
• the reinforcing layer consists of a fibrous material in the form of continuous fibers impregnated with a composition mainly comprising at least one polymer P1j , in particular an epoxy resin or based on epoxy.
• a waterproofing layer and a reinforcing layer are present and do not adhere to each other and the reinforcing layer consists of a fibrous material in the form of continuous fibers impregnated with a composition mainly comprising a polymer P1j which is an epoxy resin or epoxy-based.
• epoxy-based throughout the description means that the epoxy represents at least 50% by weight of the matrix.
• Each of said layers (a) and (b) consists of a composition predominantly comprising at least one short-chain semi-crystalline polyamide thermoplastic polymer or a long-chain semi-crystalline polyamide thermoplastic polymer.
• the short chain expression means that the polyamide has a number of carbon atoms per nitrogen atom ranging from 4 to less than 8, in particular from 6 to less than 8.
• the long chain expression means that the polyamide has a number of carbon atoms per nitrogen atom greater than or equal to 8, preferably greater than 9, in particular greater than 10.
• the term “predominantly” means that said at least one polymer is present in more than 50% by weight relative to the total weight of the composition.
• said at least one majority polymer is present at more than 60% by weight, in particular at more than 70% by weight, particularly at more than 80% by weight, more particularly greater than or equal to 90% by weight relative to the total weight of the composition.
• Said composition of layer (a) when the polyamide is long chain can also comprise up to 50% by weight relative to the total weight of the composition of impact modifiers and / or up to 3% by weight of plasticizer and / or up to 5% additives.
• the additives can be selected from another polymer, an antioxidant, a heat stabilizer, a UV absorber, a light stabilizer, a lubricant, an inorganic filler, a flame retardant, a colorant, carbon black and carbonaceous nanofillers, with the exception of a nucleating agent, in particular the additives are chosen from an antioxidant, a heat stabilizer, a UV absorber, a light stabilizer, a lubricant, an inorganic filler, a flame retardant, a colorant, carbon black and carbonaceous nanofillers, except for a nucleating agent.
• Said other polymer can be another semi-crystalline thermoplastic polymer or a different polymer and in particular an EVOH (Ethylene vinyl alcohol).
• EVOH Ethylene vinyl alcohol
• said composition of layer (a) comprises said thermoplastic polyamide polymer with a predominantly long chain, from 0 to 50% by weight of impact modifier, in particular from 0 to less than 15% of impact modifier, in particular from 0 to 12% of impact modifier, from 0 to 3% of plasticizer and from 0 to 5% by weight of additives, the sum of the constituents of the composition being equal to 100%.
• said composition of layer (a) consists of said thermoplastic polyamide polymer with a predominantly long chain, from 0 to 50% by weight of impact modifier, in particular from 0 to less than 15% of impact modifier, in particular from 0 to 12 % impact modifier, 0 to 3% plasticizer and 0 to 5% by weight of additives, the sum of the constituents of the composition being equal to 100%.
• only one major polymer is present in the sealant layer.
• said composition of layer (a) comprises an impact modifier of 0.1 to 50% by weight, in particular from 0.1 to less than 15% by weight, in particular from 0.1 to 12% by weight of impact modifier relative to the total weight of the composition. In one embodiment, said composition of layer (a) is devoid of plasticizer.
• said composition of layer (a) comprises an impact modifier from 0.1 to 50% by weight, in particular from 0.1 to less than 15% by weight, in particular from 0.1 to 12% by weight. % by weight of impact modifier and said composition of layer (a) is devoid of plasticizer relative to the total weight of the composition.
• said composition of layer (a) comprises an impact modifier from 0.1 to 50% by weight, in particular from 0.1 to less than 15% by weight, and from 0.1 to 1 5% by weight of plasticizer relative to the total weight of the composition.
• Said composition of layer (a) when the polyamide is short chain also comprises more than 15% by weight and up to 50% by weight of impact modifier relative to the total weight of the composition and / or up to 3% by weight. weight of plasticizer and / or up to 5% additives.
• the additives can be selected from another polymer, an antioxidant, a heat stabilizer, a UV absorber, a light stabilizer, a lubricant, an inorganic filler, a flame retardant, a colorant, carbon black and carbonaceous nanofillers, with the exception of a nucleating agent, in particular the additives are chosen from an antioxidant, a heat stabilizer, a UV absorber, a light stabilizer, a lubricant, an inorganic filler, a flame retardant, a colorant, carbon black and carbonaceous nanofillers, except for a nucleating agent.
• Said other polymer can be another semi-crystalline thermoplastic polymer or a different polymer and in particular an EVOH (Ethylene vinyl alcohol).
• EVOH Ethylene vinyl alcohol
• said composition of layer (a) comprises said predominantly short-chain polyamide thermoplastic polymer, from more than 15% to 50% by weight of impact modifier, in particular from 20% by weight to 50% of impact modifier, in particular of 30% by weight to 40% by weight of impact modifier, from 0 to 3% of plasticizer and from 0 to 5% by weight of additives, the sum of the constituents of the composition being equal to 100%.
• said composition of layer (a) consists of said predominantly short-chain thermoplastic polyamide polymer, from more than 15% to 50% by weight of impact modifier, in particular from 20% by weight to 50% of impact modifier, from 0 3% plasticizer and 0 to 5% by weight of additives, the sum of the constituents of the composition being equal to 100%.
• only one major polymer is present in the sealant layer.
• said composition of layer (a) comprises an impact modifier of more than 15% to 50% by weight of impact modifier, in particular from 20% by weight to 50% of impact modifier, relative to the total weight of the composition.
• said composition of layer (a) is devoid of plasticizer.
• said composition of layer (a) comprises an impact modifier of 0.1 to 50% by weight, in particular from 0.1 to less than 15% by weight, in in particular from 0.1 to 12% by weight of impact modifier and said composition of layer (a) is devoid of plasticizer relative to the total weight of the composition.
• said composition of layer (a) comprises an impact modifier from 0.1 to 50% by weight, in particular from 0.1 to less than 15% by weight, and from 0.1 to 1 5% by weight of plasticizer relative to the total weight of the composition.
• layer (b) it has the same characteristics as detailed above for layer (a) whether it is short-chain polyamide or long-chain polyamide.
• the polyamide of layer (a) and that of layer (b) can be identical or different, in particular they are identical.
• thermoplastic polyamide polymer or semi-crystalline thermoplastic polyamide polymer is understood to mean a material which is generally solid at room temperature, and which softens during an increase in temperature, in particular after passing its glass transition temperature (Tg), and which may present a clear melting on passing of its so-called melting temperature (Tm), and which becomes solid again when the temperature drops below its crystallization temperature.
• Tg, Te and Tf are determined by differential scanning calorimetry (DSC) according to standard 11357-2: 2013 and 11357-3: 2013 respectively.
• the number-average molecular mass Mn of said semi-crystalline polyamide thermoplastic polymer is preferably in a range from 10,000 to 85,000, in particular from 10,000 to 60,000, preferably from 10,000 to 50,000, even more preferably from 12,000 to 50,000. These Mn values may correspond to inherent viscosities greater than or equal to 0.8 as determined in m-cresol according to ISO 307: 2007 but by changing the solvent (use of m-cresol instead of sulfuric acid and the temperature being 20 ° C).
• the polyamide can be a homopolyamide or a copolyamide or a mixture thereof.
• said thermoplastic polymer is a long-chain aliphatic polyamide, that is to say a polyamide having an average number of carbon atoms per nitrogen atom greater than or equal to 8, preferably greater than 9, in particular greater than 10.
• the long chain aliphatic polyamide is chosen from: polyamide 11 (PA11), polyamide 12 (PA12), polyamide 1010 (PA1010), polyamide 1012 (PA1012), polyamide 1212 (PA1012), or a mixture thereof or a copolyamide thereof, in particular PA11 and PA12.
• polyamide 11 PA11
• PA12 polyamide 12
• PA1012 polyamide 1012
• PA1012 polyamide 1212
• PA1012 polyamide 1212
• PA1012 polyamide 1212
• the long chain aliphatic polyamide is chosen from: polyamide 12 (PA12), polyamide 1010 (PA1010), polyamide 1012 (PA1012), polyamide 1212 (PA1012), or a mixture of these- ci or a copolyamide thereof, in particular PA12.
• the long chain aliphatic polyamide is selected from: polyamide 12 (PA12), polyamide 1012 (PA1012), polyamide 1212 (PA1012), or a mixture of these or a copolyamide of those here, in particular PA12.
• said thermoplastic polymer is a short-chain aliphatic polyamide, that is to say a polyamide having a number of carbon atoms per nitrogen atom of from 4 to less than 8, in particular of 6 to less than 8.
• the short-chain aliphatic polyamide is chosen from PA6, PA66 and PA6 / 66.
• soldering elements made of thermoplastic polyamide polymer.
• thermoplastic polyamide polymer it can be used heated blades with or without contact, ultrasound, infrared, application of vibrations, a rotation of one element to be welded against the other or even laser welding.
• the impact modifier can be any impact modifier from the moment when a polymer of lower modulus than that of the resin, exhibiting good adhesion with the matrix, so as to dissipate the cracking energy.
• the impact modifier is advantageously constituted by a polymer having a flexural modulus of less than 100 MPa measured according to the ISO 178 standard and of Tg less than 0 ° C (measured according to the 11357-2 standard at the inflection point of the DSC thermogram ), in particular a polyolefin.
• PEBAs are excluded from the definition of impact modifiers.
• the polyolefin of the impact modifier can be functionalized or non-functionalized or be a mixture of at least one functionalized and / or at least one non-functionalized.
• the polyolefin has been designated by (B) and functionalized polyolefins (B1) and unfunctionalized polyolefins (B2) have been described below.
• An unfunctionalized polyolefin (B2) is conventionally a homopolymer or copolymer of alpha olefins or diolefins, such as, for example, ethylene, propylene, butene-1, octene-1, butadiene.
• alpha olefins or diolefins such as, for example, ethylene, propylene, butene-1, octene-1, butadiene.
• LLDPE linear low density polyethylene, or linear low density polyethylene
• VLDPE very low density polyethylene, or very low density polyethylene
• metallocene polyethylene metallocene polyethylene
• ethylene / alpha-olefin copolymers such as ethylene / propylene, EPR (abbreviation of ethylene-propylene-rubber) and ethylene / propylene / diene (EPDM).
• EPR abbreviation of ethylene-propylene-rubber
• EPDM ethylene / propylene / diene
• SEBS ethylene-butene / styrene
• SBS styrene / butadiene / styrene
• SIS styrene / isoprene / styrene
• SEPS styrene / ethylene-propylene / styrene
• the functionalized polyolefin (B1) can be a polymer of alpha olefins having reactive units (the functionalities); such reactive units are acid, anhydride or epoxy functions.
• polyolefins (B2) grafted or co- or ter polymerized with unsaturated epoxides such as glycidyl (meth) acrylate, or with carboxylic acids or the corresponding salts or esters such as (meth) acrylic acid (the latter being able to be totally or partially neutralized by metals such as Zn, etc.) or alternatively by carboxylic acid anhydrides such as maleic anhydride.
• a functionalized polyolefin is for example a PE / EPR mixture, the weight ratio of which can vary widely, for example between 40/60 and 90/10, said mixture being co-grafted with an anhydride, in particular maleic anhydride, according to a degree of grafting, for example from 0.01 to 5% by weight.
• the functionalized polyolefin (B1) can be chosen from the following (co) polymers, grafted with maleic anhydride or glycidyl methacrylate, in which the degree of grafting is for example from 0.01 to 5% by weight:
• - ethylene / alpha-olefin copolymers such as ethylene / propylene, EPR (abbreviation of ethylene-propylene-rubber) and ethylene / propylene / diene (EPDM).
• EPR abbreviation of ethylene-propylene-rubber
• EPDM ethylene / propylene / diene
• SEBS ethylene-butene / styrene
• SBS styrene / butadiene / styrene
• SIS isoprene / styrene
• SEPS styrene / ethylene-propylene / styrene
• alkyl (meth) acrylate copolymers containing up to 40% by weight of alkyl (meth) acrylate;
• the functionalized polyolefin (B1) can also be chosen from ethylene / propylene copolymers predominantly in propylene grafted with maleic anhydride then condensed with mono-amine polyamide (or a polyamide oligomer) (products described in EP-A-0342066) .
• the functionalized polyolefin (B1) can also be a co- or ter polymer of at least the following units: (1) ethylene, (2) alkyl (meth) acrylate or vinyl ester of saturated carboxylic acid and (3) anhydride such as maleic anhydride or (meth) acrylic acid or epoxy such as glycidyl (meth) acrylate.
• (meth) acrylic acid can be salified with Zn or Li.
• alkyl (meth) acrylate in (B1) or (B2) denotes methacrylates and acrylates of C1 to C8 alkyl, and may be chosen from methyl acrylate, ethyl acrylate , n-butyl acrylate, isobutyl acrylate, ethyl-2-hexyl acrylate, cyclohexyl acrylate, methyl methacrylate and ethyl methacrylate.
• the aforementioned polyolefins (B1) can also be crosslinked by any suitable process or agent (diepoxy, diacid, peroxide, etc.); the term functionalized polyolefin also includes mixtures of the aforementioned polyolefins with a difunctional reagent such as as diacid, dianhydride, diepoxy, etc. capable of reacting with these or mixtures of at least two functionalized polyolefins capable of reacting with each other.
• a difunctional reagent such as as diacid, dianhydride, diepoxy, etc.
• copolymers mentioned above, (B1) and (B2) can be copolymerized in a random or block fashion and have a linear or branched structure.
• the molecular weight, the MFI number, the density of these polyolefins can also vary to a large extent, which will be appreciated by those skilled in the art.
• MFI short for Melt Flow Index, is the melt flow index. It is measured according to standard ASTM 1238.
• the unfunctionalized polyolefins (B2) are chosen from homopolymers or copolymers of polypropylene and any homopolymer of ethylene or copolymer of ethylene and of a comonomer of higher alpha olefinic type. such as butene, hexene, octene or 4-methyl 1-Pentene.
• PPs high density PE, medium density PE, linear low density PE, low density PE, very low density PE.
• polyethylenes are known to those skilled in the art as being produced according to a “radical” process, according to a “Ziegler” type catalysis or, more recently, according to a so-called “metallocene” catalysis.
• the functionalized polyolefins (B1) are chosen from any polymer comprising alpha olefinic units and units bearing polar reactive functions such as epoxy, carboxylic acid or carboxylic acid anhydride functions.
• polymers mention may be made of the ter polymers of ethylene, of alkyl acrylate and of maleic anhydride or of glycidyl methacrylate, such as Lotader® from the Applicant or polyolefins grafted with l.
• maleic anhydride such as Orevac® from the Applicant as well as ter polymers of ethylene, of alkyl acrylate and of (meth) acrylic acid.
• Mention may also be made of homopolymers or copolymers of polypropylene grafted with a carboxylic acid anhydride and then condensed with polyamides or mono-amino polyamide oligomers.
• said constituent composition of said sealant layer or layers is devoid of polyether block amide (PEBA).
• PEBAs are therefore excluded from the impact modifiers.
• said transparent composition is devoid of core-shell particles or “core-shell” core-shell polymers.
• core-shell particle it is necessary to understand a particle of which the first layer forms the core and the second or all of the following layers form the respective shell.
• the core-shell particle can be obtained by a multi-step process comprising at least two steps. Such a method is described for example in documents US2009 / 0149600 or EP0722961. Regarding the plasticizer
• the plasticizer can be a plasticizer commonly used in compositions based on polyamide (s).
• a plasticizer which has good thermal stability so that no fumes are formed during the stages of mixing the various polymers and of processing the composition obtained.
• this plasticizer can be chosen from: benzene sulfonamide derivatives such as n-butyl benzene sulfonamide (BBSA), ortho and para isomers of ethyl toluene sulfonamide (ETSA), N-cyclohexyl toluene sulfonamide and N- (2-hydroxypropyl) benzenesulfonamide (HP-BSA), esters of hydroxybenzoic acids such as 2-ethylhexyl para-hydroxybenzoate
• BBSA n-butyl benzene sulfonamide
• ETSA ethyl toluene sulfonamide
• HP-BSA N- (2-hydroxypropyl) benzenesulfonamide
• esters of hydroxybenzoic acids such as 2-ethylhexyl para-hydroxybenzoate
• EHPB 2-decylhexyl para-hydroxybenzoate
• HDPB 2-decylhexyl para-hydroxybenzoate
• esters or ethers of tetrahydrofurfuryl alcohol such as oligoethyleneoxy-tetrahydrofurfurylalcohol
• esters of citric acid or hydroxymalonic acid such as oligoethylene oxymalonate.
• a preferred plasticizer is n-butyl benzene sulfonamide (BBSA).
• Another more particularly preferred plasticizer is N- (2-hydroxy-propyl) benzene sulfonamide (HP-BSA).
• HP-BSA N- (2-hydroxy-propyl) benzene sulfonamide
• the polymer P1j can be a thermoplastic polymer or a thermosetting polymer.
• One or more composite reinforcement layers may or may be present.
• the term “predominantly” means that said at least one polymer is present in more than 50% by weight relative to the total weight of the composition and of the matrix of the composite.
• said at least one major polymer is present at more than 60% by weight, in particular at more than 70% by weight, particularly at more than 80% by weight, more particularly greater than or equal to 90% by weight, relative to the weight total composition
• Said composition can also comprise impact modifiers and / or additives.
• the additives can be selected from an antioxidant, a heat stabilizer, a UV absorber, a light stabilizer, a lubricant, an inorganic filler, a flame retardant, a plasticizer and a colorant, except for a nucleating agent.
• said composition consists of said thermoplastic polymer P1j predominantly, from 0 to 15% by weight of impact modifier, in particular from 0 to 12% by weight of impact modifier, from 0 to 5% by weight of additives, the sum of constituents of the composition being equal to 100% by weight.
• Said at least one majority polymer of each layer may be identical or different.
• a single major polymer is present at least in the composite reinforcing layer and which does not adhere to the waterproofing layer.
• each reinforcing layer comprises the same type of polymer, in particular an epoxy or epoxy-based resin.
• thermoplastic or thermoplastic polymer
• Tg temperature of glass transition
• Tf melting temperature
• Tg, Te and Tf are determined by differential scanning calorimetry (DSC) according to standard 11357-2: 2013 and 11357-3: 2013 respectively.
• the number average molecular weight Mn of said thermoplastic polymer is preferably in a range of 10,000 to 40,000, preferably 10,000 to 30,000. These Mn values may correspond to inherent viscosities greater than or equal to 0.8 as determined in the m-cresol according to ISO 307: 2007 but changing the solvent (use of m-cresol instead of sulfuric acid and the temperature being 20 ° C).
• polyamides in particular comprising an aromatic and / or cycloaliphatic structure
• copolymers for example polyamide-polyethers, polyesters, copolymers, polyaryletherketones (PAEK), polyetherether ketones (PEEK), polyetherketone ketones (PEKK), polyetherketoneetherketone ketones (PEKEKK), polyimides in particular polyetherimides (PEI) or polyamide-imides (in particular PSU )sulfones, polylsulfones polyarylsulfones such as polyphenyl sulfones
• PAEK polyaryletherketones
• PEEK polyetherether ketones
• PEKK polyetherketone ketones
• PEKEKK polyetherketoneetherketone ketones
• PEI polyetherimides
• PSU polyamide-imides
• PPSU polyethersulfones
• semi-crystalline polymers are more particularly preferred, and in particular polyamides and their semi-crystalline copolymers.
• the polyamide can be a homopolyamide or a copolyamide or a mixture thereof.
• the semi-crystalline polyamides are semi-aromatic polyamides, in particular a semi-aromatic polyamide of formula X / YAr, as described in EP1505099, in particular a semi-aromatic polyamide of formula A / XT in which A is chosen from a unit obtained from an amino acid, a unit obtained from a lactam and a unit corresponding to the formula (diamine in Ca).
• (Cb diacid) with a representing the number of carbon atoms of the diamine and b representing the number of carbon atoms of the diacid, a and b each being between 4 and 36, advantageously between 9 and 18, the unit (Ca diamine) being chosen from aliphatic, linear or branched diamines, cycloaliphatic diamines and alkylaromatic diamines and the unit (Cb diacid) being chosen from aliphatic, linear or branched diacids, cycloaliphatic diacids and aromatic diacids ;
• XT denotes a unit obtained from the polycondensation of a Cx diamine and terephthalic acid, with x representing the number of carbon atoms of the Cx diamine, x being between 5 and 36, advantageously between 9 and 18, in particular a polyamide of formula A / 5T, A / 6T, A / 9T, A / 10T or A / 11 T, A being as defined above, in particular a polyamide chosen from a PA MPMDT / 6T, one PA11 / 10T, one PA 5T / 10T, one PA 11 / BACT, one PA 11 / 6T / 10T, one PA MXDT / 10T, one PA MPMDT / 10T, one PA BACT / 10T, one PA BACT / 6T, PA BACT / 10T / 6T, one PA 11 / BACT / 6T, PA 11 / MPMDT / 10T, PA 11 / B
• T corresponds to terephthalic acid
• MXD corresponds to m-xylylenediamine
• MPMD corresponds to methylpentamethylene diamine
• BAC corresponds to bis (aminomethyl) cyclohexane.
• Said semi-aromatic polyamides defined above have in particular a Tg greater than or equal to 80 ° C.
• thermosetting polymers are chosen from epoxy or epoxy-based resins, polyesters, vinyl esters and polyurethanes, or a mixture of these, in particular epoxy or epoxy-based resins.
• each composite reinforcing layer consists of a composition comprising the same type of polymer, in particular an epoxy or epoxy-based resin.
• Said composition comprising said polymer P1j may be transparent to radiation suitable for welding.
• the winding of the composite reinforcing layer around the waterproofing layer is carried out in the absence of any subsequent welding.
• the binder can be an adhesive composition as described in EP2098580, that is to say an adhesive composition comprising:
• At least one polyamide noted B having a melting point greater than or equal to 180 ° C and an average number of carbon atoms per nitrogen atom noted CB between 7 and 10, advantageously between 7.5 and 9.5 ;
• At least one polyamide denoted C having an average number of carbon atoms per nitrogen atom denoted CC of between 9 and 18, advantageously between 10 and 18; at least 50% by weight of said composition being formed from one or more polyamides chosen from polyamides A, B and C, the weighted average of the enthalpies of fusion of these polyamides within said composition being greater than 25J / g (DSC), the average number of carbon atoms per nitrogen atom of polyamides A, B and C also satisfying the following strict equation: CA ⁇ CB ⁇ CC.
• the binder can also be, for example, but without being limited to these, a composition based on 50% copolyamide 6/12 (of 70/30 ratio by weight) of Mn 16000, and 50% copolyamide 6/12 (ratio 30/70 by mass) of Mn 16000, a composition based on PP (polypropylene) grafted with maleic anhydride, known under the name of Admer QF551A from the company Mitsui, a composition based on PA610 ( of Mn 30,000, and as defined elsewhere) and of 36% of PA6 (of Mn 28,000) and of 1.2% of organic stabilizers (consisting of 0.8% of Lowinox 44B25 phenol from Great Lakes, of 0.2% of Irgafos phosphite 168 from the company Ciba, 0.2% anti-UV Tinuvin 312 from the company Ciba), a composition based on PA612 (of Mn 29000, and as defined elsewhere) and of 36% of PA6 (of Mn 28000
• barrier layer designates a layer having characteristics of low permeability and good resistance to hydrogen, that is to say that the barrier layer slows down the passage of hydrogen into the other layers of the structure. or even outside the structure.
• the barrier layer is therefore a layer that allows, above all, not to lose too much hydrogen in the atmosphere by diffusion, thus avoiding problems of explosion and ignition.
• barrier materials can be low carbon polyamides, that is to say whose average number of carbon atoms (C) relative to the nitrogen atom (N) is less than 9, preferably semi- crystalline and high-melting point, polyphthalamides and / or also non-polyamide barrier materials such as very crystalline polymers such as the copolymer of ethylene and vinyl alcohol (noted EVOH below), or even fluorinated materials functionalized such as functionalized polyvinylidene fluoride (PVDF), functionalized ethylene-tetrafluoroethylene (ETFE) copolymer, functionalized ethylene, tetrafluoroethylene and hexafluoro-propylene (EFEP) copolymer, polyphenylene sulfide (PPS) ) functionalized, functionalized polynaphthalate (PBN). Yes these polymers are not functionalized, so an intermediate binder layer can be added to ensure good adhesion within the MLT structure.
• PVDF functionalized polyvinylidene fluoride
• the EVOHs are particularly advantageous, in particular the richest in vivnyl alcohol comonomer as well as those modified impact because they make it possible to produce less fragile structures.
• barrier layer means in other words that said barrier layer is very poorly permeable to hydrogen, in particular the permeability to hydrogen at 23 ° C. is less than 75 cc.mm/m2.24h. atm at 23 ° C under 0% relative humidity (RH).
• the permeability can also be expressed in (cc.mm/m 2 .24h.Pa).
• the permeability must then be multiplied by 101325.
• Said multilayer structure therefore comprises a waterproofing layer and at least one composite reinforcing layer which is wrapped around the waterproofing layer and which may or may not adhere to each other.
• said sealing and reinforcing layer do not adhere to each other and consist of compositions which respectively comprise different polymers.
• said different polymers can be of the same type.
• the waterproofing layer consisting of a composition comprising an aliphatic polyamide
• the composite reinforcing layer consists of a composition comprising an aliphatic polyamide different from that of the waterproofing layer (for example PA11 for the layer. sealant and PA12 for the reinforcing layer or vice versa) or the composite reinforcing layer consists of a composition comprising a polyamide which is not aliphatic and which is for example a semi-aromatic polyamide so as to have of a high tg polymer as the matrix of the composite reinforcement.
• the waterproofing layer comprises from the inside to the outside: the layer (a), optionally a binder layer, the barrier layer, optionally a binder layer and the layer (b).
• Binder layers can be the same or different
• the sealant layer comprises from the inside to the outside: the layer (a), the barrier layer, a binder layer and the layer (b).
• the waterproofing layer comprises from the inside to the outside: the layer (a), a binder layer, the barrier layer, optionally a binder layer and the layer (b).
• the waterproofing layer comprises from the inside to the outside: the layer (a), a binder layer, the barrier layer and the layer (b). In one embodiment, the waterproofing layer comprises from the inside to the outside: the layer (a), optionally a binder layer, the barrier layer, a binder layer and the layer (b).
• the sealant layer comprises from the inside to the outside: the layer (a), the barrier layer, a binder layer and the layer (b).
• the sealant layer comprises from the inside to the outside: the layer (a), a binder layer, the barrier layer, a binder layer and the layer (b).
• the sealing layer may comprise one or more other layers, made of a thermoplastic polymer, below the layer (a) and one or more other layers, made of a thermoplastic polymer, above the layer ( b).
• the sealant layer is made from the inside to the outside: the layer (a), the barrier layer, a binder layer and the layer (b).
• the waterproofing layer is made up from the inside to the outside: the layer (a), a binder layer, the barrier layer, optionally a binder layer and the layer (b).
• the waterproofing layer is made from the inside to the outside: the layer (a), a binder layer, the barrier layer and the layer (b).
• the waterproofing layer consists of the interior to the exterior: the layer (a), optionally a binder layer, the barrier layer, a binder layer and the layer (b).
• the sealant layer is made from the inside to the outside: the layer (a), the barrier layer, a binder layer and the layer (b).
• the sealant layer is made up from the inside to the outside: the layer (a), a binder layer, the barrier layer, a binder layer and the layer (b).
• Said multilayer structure can include up to 10 composite reinforcement layers of different types.
• said multilayer structure comprises one, two, three, four, five, six, seven, eight, nine or ten layers of composite reinforcement.
• said multilayer structure comprises one, two, three, four or five composite reinforcement layers.
• said multilayer structure comprises one, two or three composite reinforcement layers.
• compositions which respectively comprise identical polymers consist of compositions which respectively comprise polymers of the same type.
• compositions which respectively comprise different polymers consist of compositions which respectively comprise different polymers.
• said multilayer structure comprises a sealing layer and a plurality of reinforcing layers, said reinforcing layer adjacent to the sealing layer being wrapped around said sealing layer and the other reinforcing layers being wrapped around of the directly adjacent reinforcement layer.
• said multilayer structure comprises a single waterproofing layer and a single composite reinforcing layer, said reinforcing layer being wrapped around said waterproofing layer.
• said polyamide of layers (a) and / or (b) is a short-chain aliphatic polyamide, in particular chosen from PA6, PA66 and PA6 / 66, or long-chain polyamide, in particular chosen from PA1010, PA 1012, PA 1212, PA11 and PA12, in particular PA11 and PA12, and said polymer P1j is an epoxy resin or an epoxy-based resin.
• said polyamide of layers (a) and (b) is a short-chain aliphatic polyamide, in particular chosen from PA6, PA66 and PA6 / 66, or long-chain, in particular chosen from PA1010 , PA 1012, PA 1212,
• PA11 and PA12 in particular PA11 and PA12, and said polymer P1j is an epoxy or epoxy-based resin.
• said polyamide of layer (a) is a short-chain aliphatic polyamide, in particular chosen from PA6, PA66 and PA6 / 66
• said polyamide of layer (b) is an aliphatic polyamide long chain, in particular chosen from PA1010, PA 1012, PA 1212, PA11 and PA12, in particular PA11 and PA12
• said polymer P1j is an epoxy resin or an epoxy-based resin.
• said polyamide of layer (a) is a long-chain aliphatic polyamide, in particular chosen from PA1010, PA 1012, PA 1212, PA11 and PA12, in particular PA11 and PA12, and said polyamide of layer (b) is a short-chain aliphatic polyamide, in particular chosen from PA6, PA66 and PA6 / 66, and said polymer P1j is an epoxy resin or based on epoxy.
• said polyamide of layers (a) and / or (b) is a short-chain aliphatic polyamide, in particular chosen from PA6, PA66 and PA6 / 66, or long-chain polyamide, in particular chosen from PA1010, PA 1012, PA 1212, PA11 and PA12, in particular PA11 and PA12, and said polymer P1j is a long-chain aliphatic polyamide, in particular chosen from PA1010, PA 1012, PA 1212, PA11 and PA12, in particular PA11 and PA12 , or a semi-aromatic polyamide, in particular chosen from polyamide 11 / 5T or 11 / 6T or 11 / 10T, MXDT / 10T, MPMDT / 10T and BACT / 10T.
• said polyamide of layers (a) and (b) is a short-chain aliphatic polyamide, in particular chosen from PA6, PA66 and PA6 / 66, or long-chain, in particular chosen from PA1010 , PA 1012, PA 1212,
• PA11 and PA12, in particular PA11 and PA12, and said polymer P1j is a long-chain aliphatic polyamide, in particular chosen from PA1010, PA 1012, PA 1212, PA11 and PA12, in particular PA11 and PA12, or a semi-aromatic polyamide, in particular chosen from polyamide 11 / 5T or 11 / 6T or 11 / 10T, MXDT / 10T, MPMDT / 10T and BACT / 10T.
• said polyamide of layers (a) and (b) is a short-chain aliphatic polyamide, in particular chosen from PA6, PA66 and PA6 / 66, and said polymer P1j is a long-chain aliphatic polyamide. chain, in particular chosen from PA1010, PA 1012, PA 1212, PA11 and PA12, in particular PA11 and PA12, or a semi-aromatic polyamide, in particular chosen from polyamide 11 / 5T or 11 / 6T or 11 / 10T, MXDT / 10T, MPMDT / 10T and BACT / 10T.
• said polyamide of layers (a) and (b) is a long-chain aliphatic polyamide, in particular chosen from PA1010,
• PA 1012, PA 1212, PA11 and PA12, in particular PA11 and PA12, and said polymer P1j is a long-chain aliphatic polyamide, in particular chosen from PA1010, PA 1012, PA 1212, PA11 and PA12, in particular PA11 and PA12, or a semi-aromatic polyamide, in particular chosen from polyamide 11 / 5T or 11 / 6T or 11 / 10T, MXDT / 10T, MPMDT / 10T and BACT / 10T.
• said polyamide of layer (a) is a short-chain aliphatic polyamide, in particular chosen from PA6, PA66 and PA6 / 66
• said polyamide of layer (b) is an aliphatic polyamide long chain, in particular chosen from PA1010, PA 1012, PA 1212, PA11 and PA12, in particular PA11 and PA12
• said polymer P1j is a long chain aliphatic polyamide, in particular chosen from PA1010, PA 1012, PA 1212, PA11 and PA12, in particular PA11 and PA12, or a semi-aromatic polyamide, in particular chosen from polyamide 11 / 5T or 11 / 6T or 11 / 10T, MXDT / 10T, MPMDT / 10T and BACT / 10T.
• said polyamide of layer (a) is a long-chain aliphatic polyamide, in particular chosen from PA1010, PA 1012, PA 1212, PA11 and PA12, in particular PA11 and PA12
• said polyamide of layer (b) is a short-chain aliphatic polyamide, in particular chosen from PA6, PA66 and PA6 / 66
• said polymer P1j is a long-chain aliphatic polyamide, in particular chosen from PA1010, PA 1012, PA 1212, PA11 and PA12, in particular PA11 and PA12, or a semi-aromatic polyamide, in particular chosen from polyamide 11 / 5T or 11 / 6T or 11 / 10T, MXDT / 10T, MPMDT / 10T and BACT / 10T.
• each reinforcing layer consists of a composition comprising the same type of polymer P1j, in particular an epoxy resin or an epoxy-based resin.
• the polyamide P1j is identical for all the reinforcing layers.
• said multilayer structure further comprises at least one outer layer made of a continuous fiberglass fibrous material impregnated with a transparent amorphous polymer, said layer being the outermost layer of said multilayer structure.
• Said outer layer is a second but transparent reinforcing layer which makes it possible to put an inscription on the structure.
• constituent fibers of said fibrous material they are in particular fibers of mineral, organic or plant origin.
• said fibrous material can be sized or not sized.
• Said fibrous material can therefore comprise up to 3.5% by weight of an organic material (thermosetting or thermoplastic resin type) called sizing.
• fibers of mineral origin mention may be made of carbon fibers, glass fibers, basalt or basalt-based fibers, silica fibers, or silicon carbide fibers, for example.
• fibers of organic origin mention may be made of fibers based on a thermoplastic or thermosetting polymer, such as semi-aromatic polyamide fibers, aramid fibers or polyolefin fibers, for example.
• they are based on an amorphous thermoplastic polymer and have a glass transition temperature Tg greater than the Tg of the polymer or mixture of thermoplastic polymer constituting the pre-impregnation matrix when the latter is amorphous, or greater than the Tm of the polymer or mixture of thermoplastic polymer constituting the prepreg matrix when the latter is semi-crystalline.
• they are based on a semi-crystalline thermoplastic polymer and have a melting point Tm greater than the Tg of the polymer or mixture of thermoplastic polymer constituting the prepreg matrix when the latter is amorphous, or greater than the Tm. polymer or mixture of thermoplastic polymer constituting the prepreg matrix when the latter is semi-crystalline.
• the organic fibers constituting the fibrous material during impregnation with the thermoplastic matrix of the final composite.
• the fibers of plant origin mention may be made of natural fibers based on flax, hemp, lignin, bamboo, silk, in particular spider silk, sisal, and other cellulose fibers, in particular viscose. These fibers of plant origin can be used pure, treated or else coated with a coating layer, with a view to facilitating the adhesion and the impregnation of the thermoplastic polymer matrix.
• the fibrous material can also be fabric, braided or woven with fibers.
• organic fibers can be mixed with mineral fibers to be pre-impregnated with thermoplastic polymer powder and to form the pre-impregnated fibrous material.
• the rovings of organic fibers can have several grammages. They can also have several geometries.
• the fibers constituting the fibrous material can also be in the form of a mixture of these reinforcing fibers of different geometries. Fibers are continuous fibers.
• the fibrous material is chosen from glass fibers, carbon fibers, basalt or basalt-based fibers, or a mixture of these, in particular carbon fibers.
• It is used as a wick or several wicks.
• the present invention relates to a method of manufacturing a multilayer structure as defined above, characterized in that it comprises a step of preparing the sealing layer by extrusion blow molding, by rotational molding, by injection and / or extrusion.
• said method of manufacturing a multilayer structure comprises a step of filament winding of the reinforcing layer as defined above around the sealing layer as defined above.
• Example 1 Permeability to hydrogen at 23 ° C of PA 11 liners and of a liner of the invention was tested.
• a 2mm sealing layer (liner) having five layers according to the invention constituting a tank of the invention was obtained by extrusion blow molding at a temperature suited to the nature of the various thermoplastic resins used.
• the liner has the following structure: PA11 // binder // EVOH // binder // PA11, the layers having the following respective thicknesses: (900pm // 50pm // 100pm // 50pm // 900pm).
• PA11 is a polyamide 11 of Mn (number molecular mass) 45,000.
• the melting point is 190 ° C., its enthalpy of fusion is 56 kJ / m 2 .
• the binder is a Tieflex S442® marketed by the company Arkema.
• EVOH is a 32% ethylene EVOH, type EVAL FP101B (Eval company)
• a wet filament winding process which consists in winding fibers around the liner, which fibers are previously pre-assembled. -impregnated in a bath of liquid epoxy or a bath based on liquid epoxy. The reservoir is then polymerized in an oven for 2 hours.
• the permeability of a PA11 liner and of a liner of the invention is measured according to a test which consists in sweeping the upper face of a film made of PA11 or made up of the five layers of the invention with the test gas (Hydrogen) and to measure by gas chromatography the flow which diffuses through the film in the lower part, swept by the carrier gas: nitrogen
• the permeability can also be expressed in (cc.mm/m 2 .24h.Pa). The permeability must then be multiplied by 101325.

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• Engineering & Computer Science (AREA)
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• 2020
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