Method of obtaining compositions based on carbon nanotubes and polyolefins

FIELD: chemistry.

SUBSTANCE: invention relates to method of obtaining nanocomposites based on polyolefins, used in obtaining different products, such as films, sheets, tubes, threads and fibres. Carbon nanotubes are preliminarily ground in water with addition of water-soluble polymer with concentration 0.01-0.1 wt %. After that, suspension is dispersed by ultrasound at maximal medium temperature not higher than 70° C. After that, suspension is applied on the surface of polyolefic granules and dried. Obtained granules of nanocomposite contain to 0.5 wt % of carbon tubes.

EFFECT: nanocomposite materials possess high volumetric and superficial electroconductivity, heat-conductivity and high rigidity, with simultaneous increase of tensile modulus of elasticity to 50%, and limit of tensile strength to 30%.

3 cl, 4 dwg, 3 tbl

 

The invention relates to a method for production of nanocomposites based on polyolefins used in the preparation of various products made of composite materials, including films, sheets, tubes, filaments and fibers, packaging, medical products, automotive spare parts and batteries, fittings.

Polymer nanocomposites are considered one of the most promising types of modern materials (see, for example, [E.T. Thostenson, C. Li, Chou, T.-W. Nanocomposites in context // Composites Science and Technology 65 (2005) 491-516, Jordan J., K.I. Jacob, Tannenbaum R., M.A. Sharaf, I. Jasiuk Experimental trends in polymer nanocomposites - a review // Materials Science and Engineering A 393 (2005) 1-11.; Hussain F., Hojjati, M., Okamoto M., R.E. Gorga Review article: Polymer-matrix Nanocomposites, Processing, Manufacturing, and Application: An Overview // Journal of Composite Materials 40 (2006) 1511-1575]). The scientific literature contains numerous publications on the properties of nanoparticles, stabilization, introduction to polymer matrix of different types to obtain nanocomposites. In domestic and foreign publications include information obtained positive results in the modification of polymer composites nanoparticles (increased strength, toughness, modulus of elasticity).

One of the most promising nanoscale reinforcing elements to obtain composites are carbon nanotubes (see, for example, reviews [Schulte K., F.H. Gojny, Fiedler B., Sandier J.K.W., Bauhofer W. Chapter 1. Carbon Nanotube-Renforced Polymers: a State of the Art Review / In: Polymer Composites: from Nano - to Macroscale. Springier (US), 2005. 3-23. Endo M., M.S. Strano, P.M. Ajayan Potential Applications of Carbon Nanotubes / In: Carbon Nanotubes (A. Jorio, G. Dresselhaus, M.S. Dresselhaus, Eds.) // Topics Appl. Physics 111 (2008) 13-62] and others).

Currently, the development of nanocomposites has had approximately 100 of the world's leading companies and corporations. So, for example, a manufacturer of carbon nanotubes company Nanocyl S.A. (Belgium), among other commercial products offers concentrates 2001 PP polypropylene-based content multilayer nanotubes up to 15-20 wt.%, which can be used in the manufacture of articles by injection molding or extrusion [http://www.nanocyl.com/products/industrial/plasticyl.php]. Compared with the pure polymer nanocontainers based on polypropylene (PlastiCyl 2001) with 25 wt.% nanotubes has a significantly higher volume and surface conductivity (an increase of 11-12 orders of magnitude), 20 times higher conductivity. The content of the polymer nanotubes increases rigidity, while the modulus of tensile elasticity is increased by 50%, the tensile strength by 30%, and a modulus of elasticity in bending is practically unchanged. The above characteristics suggest that concentrates nanotubes remain largely aggregated.

As you know, industrial manufactured nanomaterials (carbon nanotubes, particles of metals, their oxides and d) are highly aggregated state (nanotubes are stuck in clumps units). Thus, in industry there is a serious problem (problem) deaggregation nanotubes from lumps in their location within the composite. If not timely to share nanotubes, formed clusters (sticking together in clumps aggregates can significantly degrade the strength of the material. The use of nanomaterials as fillers in this form (sticking together in clumps of units) does not lead to the expected improvement of mechanical properties of polymer composites, but also significantly reduces the expected enhancement of the mechanical properties, since these units serve as the hub of internal stresses and sources of cracking. In this regard, the acknowledged problems of the introduction of nanomaterials in the polymer matrix are dispersing them to individual particles to enable the transmission properties of the nanoparticles with the molecules of the polymer matrix, and the distribution (polymeric matrix) for a given character [Xie X.-L., Y.-W. Mai, Zhou X.-P. Dispersion and alignment of carbon nanotubes in polymer matrix: A review // Materials Science and Engineering. 49 (2005) 89-112].

A common way to break up aggregates of nanoparticles, including carbon nanotubes, is the dispersion of nanomaterials in liquid medium [L. Vaisman, H.D. Wagner, Marom G. The role of surfactants in dispersion of carbon nanotubes // Advances in Colloid and Interface Science. 128-130 (2006) 37-46], as predstavleniya 1.

In this case, in the development of the method of separation of bundles of nanotubes (or aggregates of nanodiamonds) to isolate the individual type and prevent the re-aggregation in the liquid dispersion has two key points:

- select the type and modes of physical impact on nanomaterial;

the choice of liquid medium, wherein the dispersion.

Typically in such environments, the choice falls on Malopolskie organic solvents, solutions of surface-active substances (surfactants), some types of polymers in water or polar organic solvents [Kang Y., T.A. Taton Micelle-Encapsulated Carbon Nanotubes: A Route to Nanotube Composites // J. Am. Chem. Soc., 125 (2003) 5650-5651]. The use of organic solvents is usually less convenient reasons of fire safety, economic factors, their harmful effects on living organisms and the environment in General, therefore, it is preferable to use aqueous dispersions of surfactants and polymers.

Surfactants are strongly adsorbed on the surface of the nanoparticles, isolating them from the polar aqueous environment [X. Gong, J. Liu, S. Baskaran, Voise R.D., Young J.S. Surfactant-Assisted Processing of Carbon Nanotube / Polymer Composites // Chem. Mater. 12 (2000) 1049-1052]. Instead of the low-molecular surfactant may be offered the use of soluble polymers and copolymers [J.C. Grunlan, L. Liu, O. Regev Weak polyelectrolyte control of carbon nanotube dispersion in water // J. Colloid Interface Sci.317 (2008) 346-349].

Studied by the applicant prior art known method of obtaining modified filler for nanocomposites based on polyolefins, modified fillers and nanocomposites nanocomposite polyolefin by treatment in aqueous suspensions of natural layered silicate two modifying additives introduced sequentially at 60-80°C, first, cetyltrimethylammonium bromide, and then dichtgetimmerde, extract the resulting suspension and the subsequent separation from water and drying. The introduction of this modified filler in the polyolefin can significantly improve the strength of the nanocomposites nanocomposite (U.S. Pat. RF 2344066, IPC6B82B 3/00, C08J 3/205, C08L 23/00, C08K 9/04, C08K 3/34, C01B 33/44, C09C 1/42, publ. 20.01.2009). The disadvantages of this method are the inability of its application to obtain composites based on carbon nanotubes.

A method of obtaining a sealing composition based on liquid Thiokol by mixing. pre-cooked sealing paste and cured pastes, including dibutyl phthalate with the introduced carbon nanomodifiers including carbon nanotubes treated with ultrasound. The disadvantage of this method is the impossibility of its application to obtain compositions based on polyolefins (U.S. Pat. RF 2263699, IPC7C09K 3/10, publ. 10.1.2005).

The closest in technical essence and the achieved technical result is a method of nanomaterials on the basis of a wide range of polymers (mainly polystyrene and polycarbonate, but also including polyolefins and various carbon particles such as carbon nanotubes, by solubilization of nanotubes in chloroform using polyphenylenevinylene and ultrasonic treatment followed by mixing with a solution of the basic polymer (polycarbonate or polystyrene) in chloroform with the formation of a homogeneous solution nanocomposites nanocomposite of carbon nanotubes/polymer. From this solution prepare a homogeneous film with subsequent heating to 80-90 degrees to remove solvent.

The disadvantage of this method is that it is unsuitable for a number of stated thermoplastics, such as polyolefins, which are not soluble in chloroform or other solvents and cannot be combined in this way with functionalized carbon nanotubes (U.S. Patent 7479516 IPC7C01B 31/02, publ. 20.01.2009). Thus, the known method does not allow to achieve a technical result in relation to the polyolefins, such as polyethylene, polypropylene.

The claimed technical solution is illustrated by the following materials.

Figure 1 presents an explanation of the principle of separation of nanoaggregates to separate the s elements by mechanical impact.

Figure 2 presents the kinetic curve of stability of dispersion CNM-solvent after ULTRASONIC dispersion solutions for 15 min (1), 1 hour (2); t is the time elapsed after ULTRASONIC dispersion. Wavelength 500 nm. Content CNM 0.01 wt.%. Solvent: a mixture of acetone-ethanol (1:1 by volume).

3 shows the optical spectra of solutions in the system CNM (0.01 wt.%) - solvent immediately after ultrasonic treatment for 1 (1) or 5 (2) hours. Solvent: a mixture of acetone-ethanol (1:1 by volume).

4 shows the optical spectra of solutions in the system CNM (0.01 wt.%) - solvent, recorded immediately after ultrasonic treatment for 1 h (1) and after centrifugation with an acceleration of 10000 g for 5 min (2). Solvent: a mixture of acetone-ethanol (1:1 by volume).

Table 1 presents General characteristics CNM "Taunit".

Table 2 presents passport characteristics of samples of different grades of polypropylene.

Table 3 presents the ratio of polypropylene granules and suspensions CNM to obtain the desired content of modifier necessary in polypropylene.

The technical result, which directed the alleged invention, is to develop a method for obtaining nanocomposites based on polyolefins and carbon nanotubes with unique and unusual on the I conventional materials properties (audited figures), allows to obtain materials, created specifically for the customer with known often non-obvious properties, such as having a significantly higher bulk and surface electrical conductivity, ten times higher thermal conductivity, high stiffness, while increasing the modulus of tensile elasticity of up to 50% at the same time, the increase of tensile strength up to 30%, and a modulus of elasticity of these materials in bending does not practically change is not peculiar to the source material itself - the polyolefins and carbon nanotubes.

The technical result is achieved in that a method of obtaining compositions based on polyolefins and carbon nanotubes dispersed by ultrasonic treatment, characterized by the fact that carbon nanotubes within 0.5-1 hour mechanically triturated in water with the addition of a water-soluble polymer with a concentration of 0.01-0.1 wt.%, then the obtained suspension was dispersed by ultrasound for 30 min at a maximum temperature not higher than 70°C, and then applying it on the surface of the polyolefin granules and drying the obtained granules nanocomposites nanocomposite containing up to 0.5 wt.% carbon nanotubes, the method according to claim 1, characterized in that the polyolefin used polyethylene, polypropylene,a method according to claim 1, characterized in that as the water-soluble polymer used non-ionic polymers, polyvinyl alcohol, or polyvinylpyrrolidone or polyvinyl acetate, or polyacrylamide, the method according to claim 1, characterized in that as the water-soluble polymer used ion polymer: anionic polyacrylamide or cationic polyacrylamide.

As a modifier used carbon nanomaterials (CNM) "Taunit" production LLC Nanocenter" (Tambov). Properties used CNM, in accordance with the passport of the manufacturer, are shown in table 1.

As thermoplastic polymer used samples of polypropylene grades PP8300G, PP1525J and PP8300M production OAO NKNK, passport specifications are shown in table 2.

The method of obtaining nanocomposites nanocomposite can be carried out as follows.

For dispersion of carbon nanotubes in water was selected a number of water-soluble polymers: polyvinyl alcohol (PVA), polyacrylamide (PAA), polyvinylpyrrolidone (PVP), polyvinyl acetate (PVA) in the form of aqueous solutions. The concentration of polymer in solution was 0.01-0.1 wt.%. An estimated sample of carbon nanotubes mechanically triturated in a small volume of concentrated solution of a water-soluble polymer using a horizontal bead mill MSPM-1, provided the surrounding dispersion of the filler in the mixing of viscous fluids (velocity dispersion of 1000 rpm). One only mechanical mixing liquid media containing 0.005-0.1 wt.% CNM, does not give stable dispersions (stratification occurs in 0.25-5 hours). However, such pre-machining CNM in a liquid environment, as it facilitates the further individualization of the nanoparticles.

Liquid samples containing CNM, pre-processed on a horizontal bead mill MSPM-1, were subjected to subsequent treatment with an ultrasonic disperser of UZDN-2T (power 200 W, the working frequency of 22 kHz), providing further grinding of the nanomaterial to the required degree of dispersion. Sufficient processing time is 10-30 minutes were obtained dispersion with a content of carbon nanotubes to 1.5 wt.%.

Application of a dispersion of carbon nanoparticles on the pellets of the polyolefin produced in the following way. Polymer granules, pre-dried at a temperature of 80-110°C, was placed in a container with a lid. Then in a container of granules was added a dispersion of carbon nanotubes concentration required in the selected liquid medium. Capacity with pellet was vigorously shaken until uniform distribution of the dispersion on the surface of the polymer. Then the contents were poured in a thin layer (1-2 cm) on a metal sheet, which was placed in a drying closet for the past is the future drying. Drying was made at a temperature of 110°C.

An example of the most effective nanoparticles pellets of polyolefin made by the applicant in the laboratory the University is as follows.

The preparation of an aqueous dispersion CNM.

Pre-prepare a solution of polyacrylamide in distilled water at the rate final concentration of 1 g/L.

The original CNM "Taunit" is placed in the drum of the ball mill, filling it no more than 10% of the volume. Into the bowl add distilled water in an amount of 3 parts to 1 parts CNM. Next drum fill porcelain balls with a diameter of 1-3 cm at 1/3 volume. The drum lid and rotate using a mechanical drive for 1 hour at a rate of 1-3 turnover/S.

After completion of the process of mechanical destruction of agglomerates CNM contents of the drum washed the prepared polymer solution taken in the amount of 36 parts

The dispersion CNM to individual nanoparticles in the polymer solution.

Suspension CNM after mechanical destruction of agglomerates is placed in a container, in which is immersed the emitter of ultrasonic disperser. The dispersion is carried out at the operating frequency of 22 kHz with a power density of 2 W/cm3within 30 minutes during dispersion requires external cooling of the vessel. Maximum tempera is ur environment should not exceed 70°C.

Application suspension CNM on the surface of the granules.

Polypropylene granules are placed in a container, the surface of which is lined with fluoroplastic-4. The pellets cause the suspension of the CNM, which was subjected to ultrasonic dispersion. The number of suspensions depends on the required content of the CNM in the polymer. The contents of the tank are thoroughly mixed to a uniform distribution of the slurry on the surface of the granules.

The weight ratio of polypropylene granules and water suspension CNM to obtain the desired content of modifier necessary in polypropylene are shown in table 3.

Drying of the granules.

Drying of the granules of polypropylene coated with a suspension CNM produce a stream of hot air at a temperature not exceeding 110°C. the drying Time depends on temperature and air flow rate. The finished product is being poured into bags and used in the production of parts by injection molding, extrusion, molding or vacuum forming.

Getting products from the modified nanoparticles pellets of the polyolefin is carried out in the future by extrusion or injection molding. As polyolefins can be used in injection molding or extrusion grade polypropylene or polyethylene.

The resulting composites containing carbon nanotubes in individualized status and, uniformly distributed in the polymeric matrix. It meets the requirements of achieving high strength characteristics of the composite compared to the original polymer.

The claimed technical solution meets the criterion of "novelty", presented to the invention, because of the investigated level of technology not identified technical solutions characterized by these traits, leading to the implementation of the claimed technical result of the claimed technical solution.

The claimed technical solution meets the criterion of "inventive step", presented to the invention, since it is not obvious to a person skilled in the art in the consequence of the fact that the properties of the materials obtained on the basis of the claimed technical solution from the original polyolefin and carbon nanotubes do not coincide with the well-known in the world for professionals on the date of filing the application.

The claimed technical solution meets the criterion of "industrial applicability", as may be implemented on any appropriate facility using standard equipment known materials and technologies.

Table 1
(General characteristics CNM "Taunit")
Value
Outer diameter, nm20÷70
Inner diameter, nm5÷10
Length, mm2 or more
Total impurities % (after cleaning)up to 5 (up 1)
Bulk density, g/cm30,4÷0,6
The specific geometric surface, m2/g120÷130 or more
thermal stability, °C600

6,0-8,0
Table 2
(Passport characteristics of samples of different grades of polypropylene).
FeaturesBrand polypropylene
PP1525JPP8300GPP8300M
The melt flow index at of 2.16 kg and 230°C, g/10 min2,9-3,21,2-1,5
The variation of yield strength within the party, %, max±10±10±10
The modulus of elasticity in bending, MPa, not less than140010501100
Impact strength Izod at 23°C, j/m, not less than4550085
Impact strength Izod at -20°C, j/m, not less than-5035
Ultimate tensile strength, MPa, not less than342626
Elongation at yield, %, not less than10117
Mass fraction of volatile substances, %, no more than±0,12±0,12±0,12

Table 3
(The ratio of polypropylene granules and suspensions CNM to obtain the desired content of modifier necessary in polypropylene).
The content of the CNM in polypropylene, wt.%The amount of polypropylene partsThe amount of suspension CNM, parts
0,11004
0,21008
0,310012
0,410016
0,510020

1. The method of obtaining compositions based on polyolefins and carbon nanotubes dispersed by ultrasonic treatment, wherein the carbon nanotubes within 0.5-1 h mechanically triturated in water with the addition of a water-soluble polymer with a concentration of 0.01-0.1 wt.%, then the obtained suspension was dispersed by ultrasound for 30 min at a maximum temperature not higher than 70°C and then applying it to the surface of the polyolefin granules and drying the obtained granules nanocomposites nanocomposite, the content is asih to 0.5 wt.% carbon tubes.

2. The method according to claim 1, characterized in that the polyolefin used polyethylene, polypropylene.

3. The method according to claim 1, characterized in that as the water-soluble polymer used non-ionic polymers: polyvinyl alcohol, or polyvinylpyrrolidone or polyvinyl acetate, or polyacrylamide.

4. The method according to claim 1, characterized in that as the water-soluble polymer used ion polymer: anionic polyacrylamide or cationic polyacrylamide.



 

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48 cl, 6 dwg, 22 tbl, 13 ex

FIELD: nanotechnology.

SUBSTANCE: invention relates to the field of nano-and microsystem equipment and polymer nanocomposites and can be used to create the elements of nanoelectronics with adjustable resistance, protective and heat-removing film coating. The method of manufacturing a film consisting of a polymer matrix reinforced with a vertically oriented array of carbon nanotubes grown on a substrate includes dissolving of the polymer in a solvent to a viscosity that enables the solution to flow between the nanotubes, the formation on the substrate of the nanocomposite layer from the polymer solution by centrifugation, and the substrate is placed perpendicular to the plane of the centrifuge rotation, and heat treatment at a temperature no higher than the temperature of destruction of the polymer matrix, and the carbon nanotubes on the substrate are grown vertically to its surface with adjustment of density of the array of nanotubes.

EFFECT: method enables to eliminate adhesiveness of nanotubes and increase degree of their orientation in the volume of the polymer matrix to create resistive elements of different value, interconnections and dielectric sites in one technological cycle of technology that is compatible with the technology of microelectronics.

1 ex

Polymer composition // 2476460

FIELD: chemistry.

SUBSTANCE: invention relates to composite polymer materials based on a butadiene-acrylonitrile elastomer, which are widely used in cable production and footwear industry. The composition contains a butadiene-acrylonitrile elastomer SKN-26, polyvinyl chloride, sulphur, captax, thiuram, stearine and technical carbon. Components are in the following ratio, pts.wt: butadiene-acrylonitrile elastomer SKN-26-80, polyvinyl chloride 20, sulphur 1.8, captax 1, thiuram 0.2, stearine 0.2, technical carbon 0.1-5.37. The polymer composition is modified by technical carbon nanoparticles with average particle size of 20-30 nm, the amount of which is determined using the following formula: c=0.1en, where n=0, 1, 2, 3, 4, e=2.7. The invention can be used in producing vulcanisates with high tensile strength, tear resistance, good dynamic properties and heat-ageing resistance.

EFFECT: articles made from the composition are characterised by such vital physical properties as strength, work of adhesion, permittivity, modulus of elasticity, mechanical and dielectric losses.

9 dwg, 1 tbl, 6 ex

Rubber mixture // 2476459

FIELD: chemistry.

SUBSTANCE: invention relates to rubber mixtures based on butadiene-acrylonitrile rubber. The rubber mixture contains the following, pts.wt: butadiene-acrylonitrile rubber SKN-26-95 and polyvinyl chloride 5, sulphur 1.9, captax 1.19, thiuram 0.24, stearine 0.95, technical carbon 0.1-5.37. The amount of technical carbon is calculated using the formula c=0.1en, where n= 0,1,2,3,4, e=2.7.

EFFECT: disclosed rubber mixture has high operational characteristics: strength, longevity, modulus of elasticity, loss-angle tangent.

4 dwg, 1 tbl

Polymer composition // 2476458

FIELD: chemistry.

SUBSTANCE: invention relates to composite polymer materials based on synthetic butadiene rubber and can be used in cable and footwear industry. The polymer composition contains the following, pts.wt: butadiene rubber SKD-35 80, high-pressure polyethylene 20, sulphur 1.6, zinc oxide 2.4, santocure 0.72, stearine 0.8, technical carbon 0.1-5.37. The amount of technical carbon is calculated using the formula c= 0.1en, where n=0,1,2,3,4, e=2.7.

EFFECT: disclosed polymer composition has high operational characteristics: strength, dynamic and mechanical properties, modulus of elasticity and dielectric properties.

7 dwg,1 tbl

FIELD: chemistry.

SUBSTANCE: invention relates to an oil-field device which is a downhole tool and has an oil-field element, such an oil-field element, a method of conducting an oil-field operation and a method of modifying functionalised graphene plates. The oil-field device is a downhole tool and has an oil-field element made from a composite which contains a matrix material which contains a polymer, an elastomer or ceramic material, and a plurality of functionalised graphene plates which are dispersed in the matrix material and contain single-layer sheets and multiple-layer sheets, having surface area per unit mass of at least 300 m2/g. The method of conducting an oil-field operation involves selecting an oil-field device which is a downhole tool and has an oil-field element, at least part of which is made from said composite and using the oil-field device in the oil-field operation, as a result of which the oil-field element is exposed to the downhole conditions. The method of modifying functionalised graphene plates involves obtaining functionalised graphene plates and atom-transfer radical polymerisation thereof in order to bind the polymer to the surface of said plates.

EFFECT: obtaining polymer composites with good barrier and mechanical properties and making oil-field elements therefrom, having semiconductor and impermeable insulation on wires, cables and other electrical and electronic components.

18 cl, 3 dwg

FIELD: chemistry.

SUBSTANCE: invention relates to foamed granular composite materials based on vinyl aromatic polymers, having improved heat-insulation properties, and a method for production thereof (versions). The composite material has density of less than 40 g/l with content of closed pores of less than 60%. The material is also characterised by presence of heterophase areas consisting of materials which are partially miscible with the polymer matrix and/or cavities which are embedded inside the polymer matrix. Said cavities are gas and/or liquid cavities which mainly consist of a foaming system, and inside said heterophase areas there a non-uniformly distributed graphite material with degree of graphitisation, calculated using a Meyer-Mering formula, of at least 0.2. The polymer matrix is a synthetic thermoplastic polymer containing at least 60 wt % of the matrix with respect to total weight of a polymer obtained from a vinyl aromatic monomer. The disclosed granular materials enable to obtain foamed articles with low density, having high insulating capacity with minimum thickness of the panel and with cost comparable to commercially available products. The foamed articles satisfy self-extinction technical requirements of the B2 test according to specification DIN 4102 part 2, with reduced use of self-extinguishing filler materials.

EFFECT: improved heat-insulation properties.

33 cl, 11 dwg, 6 tbl, 39 ex

FIELD: process engineering.

SUBSTANCE: invention relates to translucent composite film for outer surfaces of windows. Proposed material 10 comprises underlayer material 11 with outer film PET layer 12 with surface processed for increase in adherence thereto and impregnated with substance absorbing UV radiation. Film layer 12 is applied onto the layer of metalised film 13. Processed surface of layer 12 is coated with sub layer of acryl polymer stabilised by UV radiation, or that of copolymer 14. Layer 14 is coated with UV-stabilised hard coating 15 composed by, at least, one aliphatic urethane oligomer with functionality of 2 and, at least, one multifunctional acrylate monomer. Note here that sub layer thickness equals that of hard coating. Outer surface of underlayer 11 may be coated with adhesive layer 16 to gluing film to the window glass. Adhesive layer is coated, in its turn, with cover film 17.

EFFECT: better resistance against aggressive weather.

17 cl, 2 dwg, 4 tbl

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