Classifications

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  • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
  • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
  • C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
  • C08J5/18—Manufacture of films or sheets
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01D—SEPARATION
  • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
  • B01D53/22—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by diffusion
  • B01D53/228—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by diffusion characterised by specific membranes
• • B—PERFORMING OPERATIONS; TRANSPORTING
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  • B01D69/12—Composite membranes; Ultra-thin membranes
  • B01D69/1212—Coextruded layers
• • B—PERFORMING OPERATIONS; TRANSPORTING
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  • B01D71/06—Organic material
  • B01D71/38—Polyalkenylalcohols; Polyalkenylesters; Polyalkenylethers; Polyalkenylaldehydes; Polyalkenylketones; Polyalkenylacetals; Polyalkenylketals
  • B01D71/381—Polyvinylalcohol
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  • 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
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  • B32B27/288—Layered products comprising a layer of synthetic resin comprising synthetic resins not wholly covered by any one of the sub-groups B32B27/30 - B32B27/42 comprising polyketones
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  • B32B5/18—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by features of a layer of foamed material
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  • B32B7/04—Interconnection of layers
  • B32B7/12—Interconnection of layers using interposed adhesives or interposed materials with bonding properties
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  • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
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• • C—CHEMISTRY; METALLURGY
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  • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
  • C08F210/00—Copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond
  • C08F210/04—Monomers containing three or four carbon atoms
  • C08F210/06—Propene
• • C—CHEMISTRY; METALLURGY
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  • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
  • C08F216/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal or ketal radical
  • C08F216/02—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal or ketal radical by an alcohol radical
  • C08F216/04—Acyclic compounds
  • C08F216/06—Polyvinyl alcohol ; Vinyl alcohol
• • C—CHEMISTRY; METALLURGY
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  • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
  • C08F216/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal or ketal radical
  • C08F216/36—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal or ketal radical by a ketonic radical
• • C—CHEMISTRY; METALLURGY
  • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
  • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
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  • C08L23/04—Homopolymers or copolymers of ethene
  • C08L23/08—Copolymers of ethene
  • C08L23/0846—Copolymers of ethene with unsaturated hydrocarbons containing atoms other than carbon or hydrogen
  • C08L23/0853—Ethene vinyl acetate copolymers
  • C08L23/0861—Saponified copolymers, e.g. ethene vinyl alcohol copolymers
• • C—CHEMISTRY; METALLURGY
  • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
  • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
  • C08L73/00—Compositions of macromolecular compounds obtained by reactions forming a linkage containing oxygen or oxygen and carbon in the main chain, not provided for in groups C08L59/00 - C08L71/00; Compositions of derivatives of such polymers
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• • C—CHEMISTRY; METALLURGY
  • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
  • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
  • C08F2800/00—Copolymer characterised by the proportions of the comonomers expressed
  • C08F2800/10—Copolymer characterised by the proportions of the comonomers expressed as molar percentages
• • C—CHEMISTRY; METALLURGY
  • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
  • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
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• • C—CHEMISTRY; METALLURGY
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  • C08J2329/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal, or ketal radical; Hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Derivatives of such polymer
  • C08J2329/02—Homopolymers or copolymers of unsaturated alcohols
  • C08J2329/04—Polyvinyl alcohol; Partially hydrolysed homopolymers or copolymers of esters of unsaturated alcohols with saturated carboxylic acids
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  • C08J2329/12—Homopolymers or copolymers of unsaturated ketones

Definitions

• the invention relates to the use of special polymers as barrier layers, in particular as barrier layers in composite materials.
• barrier layers exhibit a selective barrier to various gases, with the barrier effect to HFOs being especially good. Due to these properties, such barrier layers can positively influence the insulating and insulating properties, for example in thermally insulated pipes.
• Foams for insulation and insulation are known materials. Such foams find numerous uses, especially in thermal insulation and are thus important components in numerous applications.
• the insulating properties of foams depend on many parameters, including the composition of the cell gases.
• a well-known class of foams are the polyurethane foams (PU), which are formed from a polyol and an isocyanate.
• PU polyurethane foams
• a physical blowing agent is usually added, typically this is stirred into the polyol component and then mixed with the isocyanate in a high-pressure mixing head immediately before the metering of the two-component mixture (2K).
• This physical blowing agent is a first com ⁇ component of cell gases in PU foams.
• There is typically a certain amount of water in the polyol component a typical range would be 0.5-1.5 weight percent.
• This water has the following reactions: a) Reaction with the isocyanate to carbamic acid, which is unstable and immediately decomposes with elimination of carbon dioxide to the corresponding amine, b) reaction of the resulting amine with another isocyanate molecule to the corresponding urea. This reaction leads to the formation of further cell gases in PU foams and thus supports the foaming process. The resulting urea is advantageous for the thermal stability of the resulting foam. Details are described in Oertel et al (Polyurethanes, Gunter Oertel, 3. To ⁇ location in 1993, Hanser Verlag, p.13;. P.94).
• Hydrofluorolefine are a known class of Ver ⁇ bonds, these are hydrocarbons in strict contrast to chlorofluorocarbons (HFCs) for their lowmaschinehauspoten ⁇ tial global warming potential (GWP) known. Since HFOs are also incombustible, they are used as blowing agents, as mentioned for example in WO2016 / 094762. HFOs positively influence the insulation properties of foams.
• Polymeric materials generally have a certain permeability to permeants of all kinds (gaseous or liquid). But polymers differ significantly in the jewei ⁇ time quantity migrated a particular Permeent by a given material per unit time.
• EP2340929 describes an EVOH layer as barrier to O 2 and C0 2 .
• W092 / 13716 describes EVOH layers as a barrier to HFCs. As stated above, HFCs generally have different properties when compared to HFOs.
• Fig. 1 shows schematically the structure of a composite material according to the invention (10) on a SchaumstoffIsoltechnik (20) in cross section.
• (22) is the polymer of the insulation (20)
• (21) the HFO-containing cell gas of the insulation (20).
• the invention thus relates to the use of a polymer layer as a barrier (1) for gases, wherein the polymer of the polymer layer is a co-polymer of ethylene and vinyl alcohol or a copolymer of ethylene and carbon monoxide or a copolymer of ethylene and carbon monoxide and propylene - sums up; and wherein said gas is selected from the group of hydrofluoroolefins.
• hydrofluoolefins HFO in particular as cell gas (21) in a foam (22), are very well retained by said polymer layer (1).
• the loss of these cell gases the thermal insulation effect of this foam can be minimized in a foam ⁇ material over time can be obtained for a long period so.
• the polymer layer (1) described here has a relatively high permeability to carbon dioxide.
• the amount of carbon dioxide wel ⁇ ches example.
• PU polyurethane foam
• Diffusion barriers are known in many areas of technology, for example in the field of conduits / pipe systems.
• the barrier (1) as a layer of the barrier ⁇ det.
• the barrier may be present in a single layer or in a plurality of separate layers.
• the values for the permeability of polymeric materials vary over very wide ranges; more than the factor 10 5 .
• the criteria of whether a barrier effect exists are different for different permeants.
• the measured values for O2, 2 and CO2 are usually stated in the unit cm 3 / m 2 * day * bar. Values of less than 20 are said to have a good barrier effect, the polymer is considered impermeable. At values greater than 100 no barrier effect is present, the polymer is considered to be permeable. At values in between, the polymer is considered to be partially permeable.
• the measured values for HFO (determined according to ISO 15105-1: 2007-10), Cp (determined according to ISO 15105-2: 2003-02) and water (determined according to ISO 15105-3: 2003-01) are usually expressed in the unit ml / m 2 * day indicated. Values of less than 3 are said to have a good barrier effect, the polymer is considered impermeable. At values greater than 20 no barrier effect is present, the polymer is considered to be permeable. At values in between, the polymer is considered to be partially permeable.
• the invention also relates to the use of a polymer layer as a selective barrier (1) for gases, wherein the polymer of the polymer layer is a copolymer of ethylene and vinyl alcohol or a copolymer of ethylene and carbon monoxide or a co-polymer of ethylene and carbon monoxide and propylene as described herein; and wherein said bar ⁇ riere preferred
• the polymer layer (1) has the following diffusion coefficients:
• the layer described here also makes it possible, in an advantageous embodiment, for the diffusion of water out of the thermal insulation to be made possible. This property is particularly important for pipes / pipe systems whose medium pipe is made of plastic. Is tung tubes in such electrical connector / pipe systems, an aqueous medium transported ⁇ advantage, water from the medium can pass through the conduit into the insulation and thus the insulation capability vermin ⁇ countries and damage the foam insulation.
• the layer described here further allows for a certain permeability to CO2.
• a particularly suitable value for the CO2 Transparent ⁇ ness is in the range of 0.5 - 100 cm 3 / m 2 * day * bar.
• O2 can lead to oxidative damage of the insulating material, especially at high service temperatures such as those in plastic jacketed pipes (CMR). Therefore, cell gases should be free from O2 and their diffusion into the insulation should be avoided.
• CMR plastic jacketed pipes
• the barrier layer can be adapted accordingly to the desired request profile.
• foams to realize with a low thermal conductivity as possible and to maintain this low thermal conductivity over a long period of time the aim is to prevent the gases Sau ⁇ erstoff and nitrogen from the diffusion into the foam into it; to allow the diffusion of CO2 out of the foam; to prevent the diffusion of HFOs out of the foam.
• the better this succeeds the better self ⁇ properties has the foam.
• the combination of cell gases (21) from the group of HFOs and barrier layers (1) according to the formulas (II), (III), (IV) described here leads to particularly good, superadditive ⁇ insulating insulation properties in thermally insulated pipes. Such a positive interaction of these components is surprising.
• the barrier comprises a co-polymer of ethylene with carbon monoxide (so-called polyketones) or with vinyl alcohol (so-called ethylvinyl alcohols).
• the polymer has weight advantageously 50-100.%, Preferably 80-100.%, Struktureinhei ⁇ th formulas (II) or the formula (III).
• the polymer contains from 90 to 100% by weight of structural units of the formula (II) in which o and p are 1.
• the polymer contains from 90 to 100% by weight of structural units of the formula (III) in which q and r independently of one another are 1-20.
• the polymer of the formula comprises (II) a molecular weight Mw of more than 20 "000, in particular 50 ⁇ 000-500 ⁇ 000, on In one embodiment, the polymer of formula (III) has a molecular weight Mw of more than 20". 000, in particular 50 "000-500000 on.
• the polymer of the formula (II) or of the formula (III) has a melting temperature of more than 200 ° C. (measured with DSC, 10 K / min in accordance with ISO 11357-1 / 3).
• the polymer of formula (II) or of formula (III) has a low water absorption, preferably of less than 3%, measured according to DIN EN ISO 62 ⁇ OOS-OS (saturation in water at 23 ° C.).
• Polyketones are obtainable by catalytic reaction of carbon monoxide with the corresponding alkenes, such as propene and / or ethene. Such polyketones are also referred to as aliphatic polyketones. These polymers are commercially available, for example, as polyketone copolymer (formula II) or polyketone terpolymer (formula III) from. Hyosung. Such polyketones are also commercially available under the trade name Akrotek® PK.
• PKs (II, III) show in comparison to EVOHs (IV) inferior barrier properties against O2 and N2, but also inferior barrier action against H2O and CO2.
• one or the other barrier material may be advantageous depending on the intended application. For example, if plastic pipes are used, it will be more important to allow the migration of moisture to prevent their accumulation in the PU foam. For the If medium metal pipes are used, the effect of migration from the transported warm water into the foam is not observed. In this case, it may be more important to keep the thermal conductivity of the foam as low as possible over long periods of time because the KMR pipes typically used are more likely to be used in traditional district heating, where large amounts of energy are transported and the losses must be minimized.
• the barrier comprises a polymer which contains or ethyl vinyl alcohol ⁇ stands of ethyl vinyl alcohol be.
• the polymer comprises from 50 to 100% by weight, preferably from 80 to 100% by weight, of structural units of the formula (IV)
• n 2-20.
• Geeingete EVOHs are in particular random copolymers in which the ratio m / n is 30/100 to 50/100.
• Geeingete EVOH in particular have a molecular weight Mw of about 20,000, in particular from 50 * 000 to 500,000, on.
• EVOHs are commercially available, for example as an EVAL FP series or EP series from Kuraray. These are characterized by good processability, in particular they can be very well together with the normally used jacket material polyethylene (PE) by coextrusion process because their melt viscosities and melting temperatures are in a similar range.
• PE jacket material polyethylene
• EVOHs (IV) show better barrier properties against O2 and N2 compared to PKs (II, III), but also better barrier properties against H2O and CO2. Accordingly, these are Materials particularly suitable in applications where H2O and / or CO2 is low.
• the considerations Darge ⁇ laid in connection with PK apply here correspondingly.
• Gas is selected from the group of hydrofluoroolefins (HFOs). This gas may be, for example, the cell gas (21) of a foam, in particular a SchauminsIsoltechnik (20), be. This gas can consist of HFOs or contain HFOs. Typical other components of the gas are in particular (cyclo) alkanes, CO2, ⁇ , O2, H2O.
• HFOs are known and commercially available or can be prepared by known methods. The term encompasses both compounds which comprise only carbon, hydrogen and fluorine, as well as those compounds which additionally contain chlorine (also referred to as HFCO) and in each case contain at least one unsaturated bond in the molecule. HFOs can exist as a mixture of different components or as a pure component. HFOs can furthermore be present as isomeric mixtures, in particular E / Z isomers, or as isomerically pure compounds.
• particularly suitable HFOs have a boiling point above 0 ° C.
• HFOs are selected from the group comprising compounds of the formula (I), (I),
• R 5 is H, F, Cl, CF 3 is preferably Cl, CF 3
• R 6 is H, F, Cl, CF 3 , preferably H.
• HFOs are 1233zd (e.g., Solstice LBA, Honeywell) and 1336mzz (e.g., Formacel 1100, DuPont).
• thermally insulated pipes have an improved insulating behavior when the cell gases (21) of the insulation (20) at least 10 vol%, preferably at least 30 vol%, particularly preferably at least 50 vol% HFO, and this insulation is covered by a barrier (1) as described here.
• (Cyclo) -alkanes are known as cell gas of the insulation in thermally insulated pipes.
• said alkane or cycloalkane is selected from the group comprising propane, butanes, pentanes, cyclopentane, hexanes, cyclohexane.
• the combination of (cyclo) alkane with HFO can be used to fine-tune the product properties and / or to improve the manufacturability and / or to achieve a cost reduction with acceptable quality losses.
• Said (cyclo) alkanes may be present as pure Verbin ⁇ dung or as mixtures; the aliphatic alkanes can be present as isomerically pure compounds or as isomer mixtures.
• a particularly suitable (cyclo) alkane is cyclopentane (Cp).
• Carbon dioxide This is known as the cell gas of insulation in thermally insulated pipes. It can be formed as a by-product of production or added in a defined amount.
• the CC> 2 content of a cell gas is typically less than 50 vol.%.
• Nitrogen (N2), Oxygen (O2) Due to production, components from the atmosphere / ambient air can enter the cell gas. These are essentially 2 and / or O 2, for example air. The content of these cell gases is typically less than 5 vol% at the time of manufacture.
• Water (H2O) This can be present as a gas but also as a liquid. Typically, H2O passes through condensation from the environment or by permeation from a medium-conducting element into the cell gas of an insulation. In one embodiment, therefore, the invention relates to the use as described herein, wherein the cell gas (21) is a mixture comprising 10-100 vol% HFOs and 0-50 vol% (cyclo) alkanes and 0-50 full C0 2 .
• Foam substance As mentioned above, the gas may be the cell gas (21) of a foam, in particular a foam insulation (20).
• Foams of this kind are known per se, and particularly suitable are foams which comply with the standards DIN EN 253: 2015-12 (in particular for KMR) and EN15632-1: 2009 / A1: 2014, EN15632-2: 2010 / A1: 2014 and EN15632- 3: 2010 / A1: 2014 (especially for PMR).
• the term includes rigid foams and soft foams.
• Foams may be closed cell or open cell, preferably closed cell, in particular, e.g. in standard DIN EN 253: 2015-12.
• Such foams are preferably selected from the group of polyurethanes (PU), polyisocyanurates (PIR), thermoplastic polyesters (in particular PET), thermoplastic polyolefins (in particular PE and PP).
• the invention therefore also relates to the use of a polymer layer as a barrier (1) for gases as described herein, wherein the gas is the cellular gas of a foam, characterized in that said foam (polymer (22) and cell gas (21)) satisfies the following criteria :
• PE containing 50-100 vol% 1336mzz and 0-50 vol% Cp.
• the said cell gases complement each other to 100 vol%.
• these cell glasses complement each other together with CO2 and air to 100%.
• the invention further relates to the use as described herein, wherein said polymer layer (1) is a self-supporting structural element.
• the polymer layer (1) can therefore be present as a film or as a shaped body.
• the invention further relates to the use as described herein, wherein said polymer layer (1) is part of a composite material (10).
• a composite material Such composite materials are known per se.
• said composite material (10) may have the following layer structure: thermoplastic polymer (3), optional adhesion promoter (2), polymer layer as barrier (1) as described herein, optional adhesion promoter [2 " ], optionally thermoplastic polymer (3 p Components (2) and (3) are commercially available products known to those skilled in the art.
• Thermoplastic polymer (3) A wide variety of Ther ⁇ moplasten can be used; these typically have a lower barrier effect than the layer (1).
• Thermoplastic Polmyere advantageously be (3, 3 ") selected from the group consisting of commercial PE types, such as high-density PE (HDPE), low density PE (LDPE), linear low density PE (LLDPE) may be used.
• Such substances are commercially available, for example, under the brand names Amplify TM from Dow or Admer TM from Mitsui.
• the thicknesses of the individual layers mentioned can vary over a wide range and depend inter alia on the desired barrier effect with respect to the individual permeants, furthermore on the material and finally on considerations of production and costs.
• the following values have proven to be suitable:
• the layer thickness of the polymer layer (1) is advantageously in the range from 0.01 to 1 mm, preferably in the range 0.03 to 0.5 mm, particularly preferably in the range 0.05 to 0.3 mm.
• the layer thickness of the bonding agent layer (2, 2 " ) is in each case advantageously in the range of 0.01-1 mm, preferably in the range 0.05-0.5 mm, more preferably in the range 0.1-0.3 mm.
• the layer thickness of the thermoplastic polymer (3, 3 X) lies in each case ⁇ advantageous way in the range of 0.01 - 1 mm, preferably in the range 0.05- 0.5 mm, preferably in the range 0.1-0.3 mm.
• the invention further relates to the use of a polymer as a barrier layer ⁇ (1) or a composite material (10) for gases, as described herein, in many technological fields.
• the use according to the invention is not limited to a single application; rather, it can be used in all areas where the barrier effect against HFOs is useful or desirable.
• the invention relates to the use of a polymer layer (1) as described herein or a composite material (10) as described herein
• barrier material for thermal insulation in particular for refrigerators, for pipe systems in local and district heating, for pipe systems in building cooling, for pipe systems for transporting cooled media, for pipe systems in industrial applications, for pipe systems for the transport of gases, liquids or solids;
• Thermal insulation covers in particular thermally insulated pipe systems from the group of plastic medium pipe systems (PMR) and plastic jacket pipe systems (KMR). These are used for the transport of heated or cooled media, in particular water or aqueous solutions. But also the transport of other substances and chemicals can be made possible.
• PMR plastic medium pipe systems
• KMR plastic jacket pipe systems
• Example 1 Diffusion through polymeric films:
• Cp cyclopentane
• PK Aliphatic polyketone
• EVOH copolymer of ethylene and vinyl alcohol
• PAN polyacrylonitrile
• LDPE low density polyethylene
• EVOH is a good barrier for all considered permeants.
• LDPE has virtually none Barrier effect, only in the case of water, one can speak of a partial barrier effect.
• Aliphatic PK and PAN have good barrier properties against O 2 , N 2 , HFO and Cp and partially barrier against CO2 and H2O.
• Example 2 Measurement of the cell gases of a foam after aging under different environmental conditions
• Film webs of a width of 20-30 cm were welded into bags, which had a volume of about eight liters. These bags were foamed with a PU foam containing cyclopentane as the blowing agent. After completion of the foaming process, the bags were also welded at the upper end.
• a bag was first cut open and the composition of the cell gases determined (day 0).
• the other samples were stored in two climatic chambers, in one climate chamber was a temperature of 70 ° C and a relative humidity (r. F.) of 10%, in the other chamber was a temperature of 70 ° C and a relative humidity ( r., F.) of 90%.

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