WO2014139734A1 - Matériau composite contenant des fibres hydrophiles en matière plastique - Google Patents

Matériau composite contenant des fibres hydrophiles en matière plastique Download PDF

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Publication number
WO2014139734A1
WO2014139734A1 PCT/EP2014/052283 EP2014052283W WO2014139734A1 WO 2014139734 A1 WO2014139734 A1 WO 2014139734A1 EP 2014052283 W EP2014052283 W EP 2014052283W WO 2014139734 A1 WO2014139734 A1 WO 2014139734A1
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WIPO (PCT)
Prior art keywords
surfactant
fibers
composite material
weight
alcohol
Prior art date
Application number
PCT/EP2014/052283
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English (en)
Inventor
Charles Kerobo
Roger Reinicker
Emmanuel ATTIOGBE
Thomas Chirayil
Thomas Gessner
Steve SCHAEF
Dan VOJTKO
John Randolph
Original Assignee
Construction Research & Technology Gmbh
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Publication of WO2014139734A1 publication Critical patent/WO2014139734A1/fr

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
    • C04B28/02—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing hydraulic cements other than calcium sulfates
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B16/00—Use of organic materials as fillers, e.g. pigments, for mortars, concrete or artificial stone; Treatment of organic materials specially adapted to enhance their filling properties in mortars, concrete or artificial stone
    • C04B16/04—Macromolecular compounds
    • C04B16/06—Macromolecular compounds fibrous
    • C04B16/0616—Macromolecular compounds fibrous from polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • C04B16/0625—Polyalkenes, e.g. polyethylene
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B20/00—Use of materials as fillers for mortars, concrete or artificial stone according to more than one of groups C04B14/00 - C04B18/00 and characterised by shape or grain distribution; Treatment of materials according to more than one of the groups C04B14/00 - C04B18/00 specially adapted to enhance their filling properties in mortars, concrete or artificial stone; Expanding or defibrillating materials
    • C04B20/0048—Fibrous materials
    • C04B20/0068—Composite fibres, e.g. fibres with a core and sheath of different material
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00—General methods for the manufacture of artificial filaments or the like
    • D01F1/02—Addition of substances to the spinning solution or to the melt
    • D01F1/10—Other agents for modifying properties
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/02—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D01F6/04—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds from polyolefins
    • D01F6/06—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds from polyolefins from polypropylene

Definitions

  • the present disclosure generally relates to a composite material including a plurality of fibers and a method of forming the composite material. More specifically, the plurality of fibers includes a particular plastic component and a surfactant.
  • Fibers formed from thermoplastic materials tend to be chemically inert, fairly thermally stable, and have high tensile strengths which are ideal for reinforcing composite materials.
  • these reinforced composite materials typically have improved physical properties such as improved tensile strength, improved load bearing capacity, and shrinkage and crack reduction.
  • fibers typically have ordered structures and lack polar functionalities, they can exhibit undesirable hydrophobic characteristics in the composite materials which can result in poor ductility and flexural capacity. These undesirable hydrophobic characteristics typically result in poor adhesion between the fibers and the cementitious composition thereby resulting in the composite material also having undesirable properties such as brittleness and a propensity for cracking.
  • the present disclosure provides a composite material including a cementitious composition.
  • the composite material further includes a plurality of fibers disposed in the cementitious composition.
  • Each of the plurality of fibers further includes a surfactant heterogeneous ly dispersed throughout each of the plurality fibers.
  • the surfactant includes an alcohol alkoxylate, an alcohol block/heteric alkoxylate, a polyoxyethylene/polyoxypropylene block/heteric copolymer, a fatty alcohol, a fatty alkoxy alcohol, a polyalkylene glycol, a alkylphenol alkoxylate, or combinations thereof.
  • the present disclosure further provides a method of forming the composite material.
  • the method includes the step of combining the plastic component and the surfactant to form a plurality of fibers.
  • the method further includes the step of disposing the plurality of fibers in the cementitious composition to form the composite material.
  • Figure 1 is a image by Brightfield reflected light microscopy illustrating a cross-sectional view of one embodiment of a fiber of this disclosure including a surfactant disposed throughout the fiber.
  • Figure 2 is a line graph of tensile stress as a function of displacement of Examples 1 through 3 and Comparative Example below.
  • the present disclosure provides a composite material.
  • the composite material includes a cementitious composition.
  • the cementitious composition may be, include, or consist essentially of cement, concrete, mortar, or combinations thereof.
  • the terminology "consist essentially of” describes that the cementitious composition is free of other composite materials or compositions such as asphalt, etc.
  • the cementitious composition is (or is formed from) the reaction product of a hydraulic cement binder, aggregate, and water.
  • the hydraulic cement binder may be alternatively described as cement before the formation of the cementitious composition, during formation of the cementitious composition, and/or after formation of the cementitious composition.
  • Non-limiting examples of the hydraulic cement binder are or include Portland cement, Masonry cement, and/or Mortar cement.
  • the hydraulic cement binder may be present prior to the formation of the cementitious composition in an amount of from 1 to 98 part(s) by weight, of from 40 to 85 parts by weight, or of from 60 to 80 parts by weight, each based on 100 parts by weight of the cementitious composition.
  • the aggregate may include coarse and/or fine aggregate as understood in the art.
  • the aggregate may be present prior to, during, and/or after the formation of the cementitious composition in an amount of from 1 to 98 part(s) by weight, or of from 5 to 50 parts by weight, or of from 10 to 30 parts by weight, each based on 100 parts by weight of the cementitious composition.
  • the water may be present prior to, during, and/or after the formation of the cementitious composition in an amount of from 1 to 98 part(s) by weight, of from 5 to 50 parts by weight, or of from 10 to 30 parts by weight, each based on 100 parts by weight of the cementitious composition.
  • the cementitious composition may also include other materials such as limestone, hydrated lime, fly ash, blast furnace slag, silica fume, water reducers, air entrainers, accelerators, retarders, polymeric fibers different from the plurality of fibers of this disclosure, steel fibers, or combinations thereof.
  • the cementitious composition is further defined as concrete before the formation of the cementitious composition, during formation of the cementitious composition, and/or after formation of the cementitious composition.
  • Concrete may be (or be formed from) the reaction product of a hydraulic cement binder such as Portland cement, fine and/or coarse aggregate such as sand, gravel and crushed stone, and water.
  • the hydraulic cement binder, the aggregate, and the water are typically mixed thoroughly to produce a heterogeneous mixture of concrete.
  • the hydraulic cement binder and the water initially form a gel that undergoes a process of hydration. As the concrete sets, the gel can become rigid thereby fixing the aggregate and curing the concrete.
  • the hydraulic cement binder may be present prior to the formation of the concrete in an amount of from 1 to 98 part(s) by weight, of from 40 to 85 parts by weight, or of from 60 to 80 parts by weight, each based on 100 parts by weight of the concrete.
  • the aggregate may be present prior to, during, and/or after the formation of the concrete in an amount of from 1 to 98 part(s) by weight, or of from 5 to 50 parts by weight, or of from 10 to 30 parts by weight, each based on 100 parts by weight of the concrete.
  • the water may be present prior to, during, and/or after the formation of the concrete in an amount of from 1 to 98 part(s) by weight, of from 5 to 50 parts by weight, or of from 10 to 30 parts by weight, each based on 100 parts by weight of the concrete.
  • the cementitious composition is further defined as mortar.
  • Mortar may be (or be formed from) the reaction product of a hydraulic cement binder such as Portland cement, fine aggregate such as sand, and water. Formation of mortar generally follows a similar process of hydration as the concrete described above.
  • the hydraulic cement binder may be present prior to formation of the mortar in an amount of from 1 to 98 part(s) by weight, of from 40 to 85 parts by weight, or of from 60 to 80 parts by weight, each based on 100 parts by weight of the mortar.
  • the aggregate may be present prior to, during, and/or after the formation of the mortar in an amount of from 1 to 98 part(s) by weight, of from 5 to 50 parts by weight, or of from 10 to 30 parts by weight, each based on 100 parts by weight of the mortar.
  • the water may be present prior to, during, and/or after the formation of the mortar in an amount of from 1 to 98 part(s) by weight, of from 5 to 50 parts by weight, or of from 10 to 30 parts by weight, each based on 100 parts by weight of the mortar.
  • the composite material further comprises a plurality of fibers 10.
  • the terminology, "fiber(s)" may be substituted below for either "the plurality of fibers", "each of the plurality of fibers", or both.
  • the fibers 10 may be in monofilament form, collated fibrillated form, ribbon form, or any core-sheath, core-shell, mono component, or bicomponent form or any other form known in the art.
  • the fibers 10 may be of any size and/or dimension known in the art.
  • each of the plurality of fibers 10 may have a length of from 1/8 to 3 inch(es), of from 1/4 to 2 inch(es), or of from 1/2 to 1 inch.
  • each of the plurality of fibers 10 may have a diameter of from 0.01 to 2 millimeters, of from 0.03 to 1 millimeter(s), or of from 0.04 to 0.5 millimeters.
  • the plurality of fibers 10 is disposed in the cementitious composition.
  • the plurality of fibers 10 may be disposed on at least one surface of the cementitious composition or disposed within all or a portion of the cementitious composition. At least one surface of the cementitious composition may be free of the plurality of fibers 10.
  • the terminology "disposed” may be used interchangeably with the terminology “dispersed” throughout the present disclosure.
  • the plurality of fibers 10 is present in an amount of from 0.1 to 10 parts by volume based on 100 parts by volume of the composite material.
  • the plurality of fibers 10 are present in an amount of from 0.5 to 5 parts by volume, 1 to 3 part(s) by volume, or 1.5 to 2 parts by volume, each based on 100 parts by volume of the composite material.
  • Each of the plurality of fibers 10 includes a plastic component 12.
  • the plastic component 12 may be, include, consist essentially of, or consist of any plastic known in the art. For example, in one embodiment, the terminology "consists essentially of describes the plastic component 12 free of non-plastics.
  • the plastic component 12 may be provided as a solid or a liquid.
  • the plastic component 12 may be, include, consist essentially of, or consist of a homopolymer which is formed from a single repeating unit or a copolymer which is formed from a differing of repeating units.
  • the plastic component 12 may be, include, consist essentially of, or consist of a polymerization product of monomers including, but not limited to, aliphatic monomers, aromatic monomers, and combinations thereof.
  • the plastic component 12 may be, include, consist essentially of, or consist of a polymerization product of monomers including unsaturated monomers such as alkenes and dienes having carbon-carbon double bonds, alkynes having carbon-carbon triple bonds, and styrene monomers.
  • the plastic component 12 may be, include, consist essentially of, or consist of a polymer blend of homopolymers, copolymers, or combinations thereof. In certain embodiments, the plastic component 12 has an average molecular weight of at least 1 ,000 g/mol.
  • the plastic component 12 has an average molecular weight of at least 3,000 g/mol, of at least 8,000 g/mol, of at least 10,000 g/mol, of at least 12,000 g/mol, of at least 13,000 g/mol, of at least 15,000 g/mol, of at least 25,000 g/mol, of at least 50,000 g/mol, of at least 100,000 g/mol, of at least 500,000 g/mol, or of at least 1,000,000 g/mol.
  • the plastic component 12 has an average molecular weight of from 1 ,000 g/mol to 2,000,000 g/mol.
  • the plastic component 12 has an average molecular weight of from 1 ,000 g/mol to 1 ,000,000 g/mol, of from 1 ,000 g/mol to 500,000 g/mol, of from 3,000 g/mol to 100,000 g/mol, of from 3,000 g/mol to 50,000 g/mol, of from 5,000 g/mol to 25,000 g/mol, or of from 5,000 g/mol to 15,000 g/mol.
  • the plastic component 12 is, includes, consists essentially of, or consists of a polyolefin, polyolefin elastomer, polystyrene, polyvinyl chloride, or combinations thereof.
  • the terminology "consists essentially of describes that the fibers 10 are free of other organic and/or inorganic polymers.
  • the polyolefin is polyethylene, polypropylene, polymethylpentene, polybutene-1 , or combinations thereof.
  • the polyolefin elastomer is polyisobutylene, ethylene propylene rubber, ethylene propylene diene monomer rubber.
  • the generic chemical structures of polyethylene, polypropylene, polystyrene, and polyvinyl chloride are shown below:
  • n may be any integer, e.g. from 350 to 11 ,000.
  • the plastic component 12 is polypropylene.
  • the polypropylene may be isotactic, syndiotactic, or atactic.
  • atactic For descriptive purposes only, generic chemical structures of atactic, isotactic, and syndiotactic polypropylene are shown below:
  • n may be any integer.
  • a non-limiting example of a suitable polypropylene is commercially available from
  • Pro-faxTM such as Pro-faxTM 6301.
  • Each of the plurality of fibers 10 typically includes at least 90 parts by weight of the plastic component 12 based on 100 parts by weight of each of the plurality fibers 10.
  • each of the plurality of fibers 10 may include at least 92 parts by weight, at least 94 parts by weight, at least 96 parts by weight, at least 97 parts by weight, at least 98 parts by weight, or at least 99 parts by weight of the plastic component 12, each based on 100 parts by weight of each of the plurality fibers 10.
  • Each of the plurality of fibers 10 further includes a surfactant 14.
  • the surfactant 14 includes an alcohol alkoxylate, an alcohol block/heteric alkoxylate, a polyoxyethylene/polyoxypropylene block/heteric copolymer, a fatty alcohol, a fatty alkoxy alcohol, a polyalkylene glycol, a alkylphenol alkoxylate, or combinations thereof.
  • the surfactant 14 may be provided as a solid, paste, flake, and/or liquid.
  • the surfactant 14 may be, include, consist essentially of, or consist of a soap, detergent, wetting agent, dispersant, emulsifier, foaming agent, bactericide, corrosion inhibitor, anti-static agent, surface-active agent, a polymeric surfactant, a surface-active polymer, etc.
  • the terminology "consists essentially of describes the surfactant 14 free of non-surfactants.
  • the surfactant 14 may be cationic, anionic, nonionic, amphoteric, or zwitterionic. In various embodiments, the surfactant 14 is nonionic.
  • the surfactant 14 is heterogeneous ly dispersed throughout each of the plurality fibers 10. Said differently, the surfactant 14 is distributed generally or approximately evenly throughout the fiber 10 such that a cross-section of the fiber 10 shows surfactant 14 present in approximately the entirety of the cross-section (see, e.g. Figure 1).
  • the fibers 10, which include the surfactant 14 heterogeneously dispersed throughout the fiber 10 exhibit hydrophilic characteristics. These hydrophilic characteristics may improve the adhesion of the fiber 10 to the cementitious composition.
  • Composite materials which include cementitious compositions and fibers 10 having improved adhesion to the cementitious composition exhibit, for example, increased ductility. This increased ductility may resist brittleness and provide resistance to cracking.
  • the fibers 10 which include the surfactant 14 may be coated with a variety of coatings such as surfactants and/or lubricants and/or subjected to a variety of treatments such as corona, treatment, plasma treatment, flame treatment, chromium and/or acidic oxidation. However, it is to be appreciated that these coatings and/or treatments are not required.
  • the surfactant 14 has an average molecular weight of less than or equal to 100,000 g/mol.
  • the surfactant 14 may have an average molecular weight of less than or equal to 90,000 g/mol, less than or equal to 50,000 g/mol, less than or equal to 25,000 g/mol, less than or equal to 20,000 g/mol, less than or equal to 15,000 g/mol, less than or equal to 10,000 g/mol, less than or equal to 7,000 g/mol, less than or equal to 5,000 g/mol, less than or equal to 2,000 g/mol, less than or equal to 1 ,000 g/mol, or less than or equal to 500 g/mol. While it is understood that molecular weight and molar mass represent different physical properties, with regard to the surfactant 14 of the present disclosure, the molecular weight can hereinafter be used to describe both molecular weight and molar mass.
  • the surfactant 14 is an alcohol alkoxylate.
  • the alcohol alkoxylate is not particularly limited but may be an alcohol alkoxylate with a fatty alcohol moiety having the formula:
  • R is Cs to C 18 , such as C 8 , C9, C 10 , Cn, C 12 , C 13i C M , C 15 , C 16 , C 17 , or C 18 branched or straight chain alkyl group
  • m is 0 to 14, such as 0, 1 , 2, 3, 4, 5, 6, 7, 8, 9, 10, 11 , 12, 13, or 14
  • n is O to 14, such as 0, 1, 2, 3, 4, 5, 6, 7, 8, 9, 10, 11 , 12, 13, or 14,
  • 0 is 0 to 14, such as 0, 1, 2, 3, 4, 5, 6, 7, 8, 9, 10, 11 , 12, 13, or 14,
  • p is 0 to 14, such as 0, 1 , 2, 3, 4, 5, 6, 7, 8, 9, 10, 11 , 12, 13, or 14, and
  • R' is -CH 3 , -CH 2 CH 3 , and mixtures thereof
  • R" is -CH 3 , -CH 2 CH 3 , and mixture thereof
  • R'" is -OH, -CH 3 , -0-C 3 -Cis hydroxyal
  • the alcohol alkoxylate may alternatively be an alcohol with one or more fatty alcohol moiety alkoxylate having the formula:
  • R is Cs to C 18 , such as C 8 , C9, C 10 , Cn, C 12 , C 13 , CM, C 15 , C 16 , C 17 , or C 18 branched or straight chain alkyl group
  • x is 0 to 14, such as 0, 1 , 2, 3, 4, 5, 6, 7, 8, 9, 10, 1 1 , 12, 13, or 14, y 3 to 14, such as 3, 4, 5, 6, 7, 8, 9, 10, 1 1 , 12, 13, or 14, z is 0 to 20, such as 0, 1 , 2, 3, 4, 5, 6, 7, 8, 9, 10, 1 1 , 12, 13, 14, 15, 16, 17, 18, 19, or 20,
  • p is 0 to 14, such as 0, 1 , 2, 3, 4, 5, 6, 7, 8, 9, 10, 1 1 , 12, 13, or 14, and
  • R' is -CH 3 , -CH 2 CH 3 , and mixtures thereof
  • R" is -CH 3 , -CH 2 CH 3 , and mixture thereof
  • R'" is -OH, -CH 3 , -0-C 3 -C
  • the alcohol alkoxylate may alternatively be a fatty alcohol having one or more oxyethylate moieties having the formula:
  • R(OCH 2 CH 2 ) OH wherein R is C 10 to C 13 such as C 10 , Cn, C 12 , or C 13 branched or straight chain alkyl group, and x is 4 to 10, such as 4, 5, 6, 7, 8, 9, or 10.
  • the alcohol alkoxylate is typically nonionic, but may be cationic, anionic, amphoeric or zwitterionic.
  • the alcohol alkoxylate may have a degree of ethoxylation of from 1 to 100.
  • the alcohol alkoxylate may have a degree of ethoxylation of from 20 to 100, of from 40 to 100, of from 60 to 100, or of from 70 to 90.
  • An increase in the degree of ethoxylation may increase the adhesion of the fiber 10 to the cementitious composition.
  • the alcohol alkoxylate has an average molecular weight of from 500 to 10,000 g/mol.
  • the alcohol alkoxylate has an average molecular weight of from 1 ,000 to 10,000 g/mol, of from 2,000 to 4,500 g/mol, of from 2,500 to 4,000 g/mol, or of from 3,000 to 4,000 g/mol.
  • a non- limiting example of a suitable alcohol alkoxylate is commercially available from BASF Corporation of Florham Park, J.
  • the surfactant 14 is an alcohol block/heteric alkoxylate. In other embodiments, the surfactant 14 is a polyoxyethylene/polyoxypropylene block/heteric copolymer (EO/PO block/heteric copolymer).
  • EO/PO block/heteric copolymer polyoxyethylene/polyoxypropylene block/heteric copolymer
  • the EO/PO block/heteric copolymer may be any block or heteric/block polyoxyalkylene polymer for example having the formula:
  • Y is the nucleus of an active hydrogen containing organic compound having a functionality of x from 1 to 6, such as 1, 2, 3, 4, 5, or 6 and (i) 2 to 6 carbon atoms, such as 2, 3, 4, 5, or 6 carbon atoms and 2 to 3 reactive hydrogen atoms or (ii) 6 to 18 carbon atoms, such as 6, 7, 8, 9 ,10, 11 , 12, 13, 14, 15, or 16, 17, or 18 carbon atoms and 1 to 3 reactive hydrogen atoms, such as 1 , 2, or 3 reactive hydrogen atoms.
  • A is typically a lower alkylene oxide selected from the group consisting of propylene oxide, butylene oxide, tetrahydrofuran or mixtures thereof.
  • Up to 25 percent by weight, up to 20 percent by weight, up to 15 percent by weight, up to 10 percent by weight, or up to 5 percent by weight of A may be reacted directly with the active hydrogen containing organic compound in admixture with ethylene oxide, 75 percent by weight or more, 80 percent by weight or more, 85 percent by weight or more, 90 percent by weight or more, or 95 percent by weight or more of A may be subsequently reached to produce the polymer.
  • m may be 0 to 1 10, such as 0, 1 , 2, 3, 4, 5, 6, 7, 8, 9, 10, 1 1 , 12, 13, 14, 15, 16, 17, 18, 19, 20, 21, 22, 23, 24, 25, 26, 27, 28, 29, 30, 31, 32, 33, 34, 35, 36, 37, 38, 39, 40, 41, 42, 43, 44, 45, 46, 47, 48 ,49, 50, 51, 52, 53, 54, 55, 56 ,57, 58, 59, 60, 61, 62, 63, 64, 65, 66, 67, 68, 69, 70, 71, 72, 73, 74, 75, 76, 77, 78, 79, 80, 81, 82, 83, 84, 85, 86, 87, 88, 89, 90, 91, 92, 93,94, 95,96,97,98,99, 100, 101, 102, 103, 104, 105, 106, 107, 108, 109, or 110.
  • N may be 0 to 26, such
  • the EO/PO block/heteric copolymer may also be a block or heteric/block polyoxyalkylene polymer having the formula:
  • Y is the nucleus of an active hydrogen containing organic compound having a functionality of x from 1 to 6, such as 1,2, 3, 4, 5, or 6 and (i) 2 to 6 carbon atoms, such as 2, 3, 4, 5, or 6 carbon atoms and 2 to 3 reactive hydrogen atoms or (ii) 6 to 18 carbon atoms, such as 6, 7, 8, 9 ,10, 11, 12, 13, 14, 15, or 16, 17, or 18 carbon atoms and 1 to 3 reactive hydrogen atoms, such as 1, 2, or 3 reactive hydrogen atoms.
  • A is typically a lower alkylene oxide selected from the group consisting of propylene oxide, butylene oxide, tetrahydrofuran or mixtures thereof. Up to 25 percent by weight, up to 20 percent by weight, up to 15 percent by weight, up to 10 percent by weight, or up to 5 percent by weight of A may be reacted directly with the active hydrogen containing organic compound in admixture with ethylene oxide, 75 percent by weight or more, 80 percent by weight or more, 85 percent by weight or more, 90 percent by weight or more, or 95 percent by weight or more of A may be subsequently reached to produce the polymer.
  • m may be 0 to 110, such as 0, 1, 2, 3, 4, 5, 6, 7, 8, 9, 10, 11, 12, 13, 14, 15, 16, 17, 18, 19, 20, 21, 22, 23, 24, 25, 26, 27, 28, 29, 30, 31, 32, 33, 34, 35, 36, 37, 38, 39, 40, 41, 42, 43, 44, 45, 46, 47, 48 ,49, 50, 51, 52, 53, 54, 55, 56 ,57, 58, 59, 60, 61, 62, 63, 64, 65, 66, 67, 68, 69, 70, 71, 72, 73, 74, 75, 76, 77, 78, 79, 80, 81, 82, 83, 84, 85, 86, 87, 88, 89, 90, 91, 92, 93, 94, 95,96, 97,98, 99, 100, 101, 102, 103, 104, 105, 106, 107, 108, 109, or 110.
  • N may be 0 to 26, such as 0, 1,2,3,4,5,6, 7,8,9, 10, 11, 12, 13, 14, 15, 16, 17, 18, 19,20,21,22,23,24, 25, or 26.
  • O may be 0 to 26, such as 0, 1,2, 3,4,5,6,7,8,9, 10, 11, 12, 13, 14, 15, 16, 17, 18, 19,20,21,22,23,24, 25, or 26.
  • the EO/PO block/heteric copolymer may alternatively be a block or heteric/block polyoxyalkylene polymer having the formula:
  • Y[(A) 0 (EO/A) ra (A) occasionHL wherein Y is the nucleus of an active hydrogen containing organic compound having a functionality of x from 1 to 6, such as 1,2, 3, 4, 5, or 6, and (i) 2 to 6 carbon atoms, such as 2, 3, 4, 5, or 6 carbon atoms and 2 to 3 reactive hydrogen atoms or (ii) 6 to 18 carbon atoms, such as 6, 7, 8, 9 ,10, 11, 12, 13, 14, 15, or 16, 17, or 18 carbon atoms and 1 to 3 reactive hydrogen atoms, such as 1, 2, or 3 reactive hydrogen atoms.
  • A is typically a lower alkylene oxide selected from the group consisting of propylene oxide, butylene oxide, tetrahydrofuran or mixtures thereof.
  • Up to 25 percent by weight, up to 20 percent by weight, up to 15 percent by weight, up to 10 percent by weight, or up to 5 percent by weight of A may be reacted directly with the active hydrogen containing organic compound in admixture with ethylene oxide, 75 percent by weight or more, 80 percent by weight or more, 85 percent by weight or more, 90 percent by weight or more, or 95 percent by weight or more of A may be subsequently reached to produce the polymer.
  • m may be 0 to 110, such as 0, 1, 2, 3, 4, 5, 6, 7, 8, 9, 10, 11, 12, 13, 14, 15, 16, 17, 18, 19, 20, 21, 22, 23, 24, 25, 26, 27, 28, 29, 30, 31, 32, 33, 34, 35, 36, 37, 38, 39, 40, 41, 42, 43, 44, 45, 46, 47, 48 ,49, 50, 51, 52, 53, 54, 55, 56 ,57, 58, 59, 60, 61, 62, 63, 64, 65, 66, 67, 68, 69, 70, 71, 72, 73, 74, 75, 76, 77, 78, 79, 80, 81, 82, 83, 84, 85, 86, 87, 88, 89, 90, 91, 92, 93, 94, 95,96, 97,98, 99, 100, 101, 102, 103, 104, 105, 106, 107, 108, 109, or 110.
  • N may be 0 to 26, such as 0, 1 , 2, 3, 4, 5, 6, 7, 8, 9, 10, 11 , 12, 13, 14, 15, 16, 17, 18, 19, 20, 21, 22, 23, 24, 25, or 26.
  • O may be 0 to 26, such as 0, 1 , 2, 3, 4, 5, 6, 7, 8, 9, 10, 1 1, 12, 13, 14, 15, 16, 17, 18, 19, 20, 21, 22, 23, 24, 25, or 26.
  • the EO PO block/heteric copolymer is typically nonionic, but may be cationic, anionic, amphoteric or zwitterionic.
  • the EO/PO block/heteric copolymer may terminate in a primary hydroxyl group, but may be different.
  • the EO/PO block/heteric copolymer is formed from repeating units polyethylene oxide and polypropylene oxide. The polyethylene oxide contributes to the degree of ethoxylation of the EO/PO block/heteric copolymer which, as described above, may increase the adhesion of the fiber 10 to the cementitious composition.
  • the EO/PO block/heteric copolymer has an average molecular weight of from 5,000 to 15,000 g/mol.
  • the EO/PO block/heteric copolymer may have an average molecular weight of from 5,500 to 14,000 g/mol, of from 6,000 to 13,500 g/mol, of from 6,500 to 13,000 g/mol, or of from 7,000 to 13,000 g/mol.
  • the surfactant 14 is a fatty alcohol. In other embodiments, the surfactant 14 is a fatty alkoxy alcohol. In still other embodiments, the surfactant 14 is a poly polyalkylene glycol.
  • the surfactant 14 is an alkylphenol alkoxylate.
  • the alkylphenol alkoxylate is not particularly limited but may be an alkyl phenol alkoxylate having the formula:
  • Each of the plurality of fibers 10 typically includes less than or equal to 10 parts by weight of the surfactant 14 based on 100 parts by weight of each of the plurality of fibers 10.
  • each of the plurality of fibers 10 may include less than or equal to 8 parts by weight, less than or equal to 6 parts by weight, less than or equal to 4 parts by weight, less than or equal to 3 parts by weight, less than or equal to 2 parts by weight, or less than or equal to 1 parts by weight of the surfactant 14, each based on 100 parts by weight of each of the plurality of fibers 10.
  • Each of the plurality of fibers 10 may also include one or more additives.
  • the additives may be antioxidants and/or light stabilizers.
  • the antioxidant may be or include a first and/or a second antioxidant.
  • the fiber may include any number of antioxidants.
  • the light stabilizer may be or include hindered amine light stabilizers (HALS).
  • HALS hindered amine light stabilizers
  • the first antioxidant may be present in the plurality of the fibers in an amount of from 0.001 to 1 part(s) by weight, of from 0.01 to 0.2 parts by weight, or of from 0.05 to 0.15 parts by weight, each based on 100 parts by weight of each of the plurality of fibers 10.
  • a non-limiting example of a suitable primary antioxidant is commercially available from BASF Corporation of Florham Park, NJ, under the trade name of Irganox ® , such as Irganox ® 3114 (AO) and Irganox ® B 1411 (AO).
  • the second antioxidant may be present in the plurality of fibers in an amount of from 0.001 to 1 part(s) by weight, of from 0.01 to 0.2 parts by weight, or of from 0.05 to 0.15 parts by weight, each based on 100 parts by weight of each of the plurality of fibers 10.
  • a non-limiting example of a suitable secondary antioxidant is commercially available from BASF Corporation of Florham Park, NJ, under the trade name of Irgafos ® , such as Irgafos ® 168 (AO).
  • the light stabilizer may be present in the plurality of fibers in an amount of from 0.01 to 2 parts by weight, of from 0.08 to 1 part(s) by weight, or of from 0.1 to 0.3 parts by weight, each based on 100 parts by weight of each of the plurality of fibers 10.
  • a non-limiting example of a suitable light stabilizer is commercially available from BASF Corporation of Florham Park, NJ, under the trade name of Chimassorb ® , such as Chimassorb ® 2020.
  • the fibers 10 which include the surfactant 14 may exhibit hydrophilic characteristics. Hydrophilicity may be evaluated by determining the water absorption of the fiber 10. A greater water absorption of the fibers 10 generally indicates that the fibers 10 have increased hydrophilicity.
  • a fiber 10 having a length of 90 meters may be first weighed to ascertain the "dry weight" of fiber 10. Next, the fiber 10 may be immersed in water for one minute. The fiber 10 may then removed from the water and then hung for two minutes to remove any excess water. Finally, the fiber 10 may be weighed again to ascertain the "wet weight" of fiber 10. The water absorption of the fiber 10 may then be calculated by using the following formula:
  • Each of the plurality of fibers 10 may exhibit a water absorption of at least 50 parts by weight of water based on 100 parts by weight of each of the plurality of fibers 10.
  • each of the plurality of fibers 10 may exhibit a water absorption of at least 60 parts by weight of water, of at least 70 parts by weight of water, of at least 80 parts by weight of water, of at least 90 parts by weight of water, of at least 100 parts by weight of water, of at least 150 parts by weight of water, of at least 200 parts by weight of water, of at least 300 parts by weight of water, of at least 400 parts by weight of water, or of at least 500 parts by weight of water, each based on 100 parts by weight of each of the plurality of fibers 10.
  • each of the plurality of fibers 10 may exhibit a water absorption of from 60 parts by weight to 500 parts by weight, of from 70 parts by weight to 450 parts by weight, or of from 80 parts by weight to 400 parts by weight, each based on 100 parts by weight of each of the plurality of fibers 10.
  • Hydrophilicity may also be evaluated by determining the contact angle that water exhibits with the fiber 10.
  • the surfactant 14 may lower the interfacial tension between water and the fiber 10 thereby permitting the water to "wet" the fiber 10.
  • wetting describes the ability of a liquid to maintain contact with a solid resulting from intermolecular interactions when the liquid and solid are combined.
  • water that may be added to or during formation of the cementitious composition for hydration may be able to wet the fiber 10 which includes the surfactant 14 thereby increasing adhesion of the fiber 10 to the cementitious composition.
  • This "wetting" of the fiber 10 may be evaluated by determining the contact angle that water exhibits with a molded sheet, formed from the plastic component 12 and the surfactant 14. Typically, the contact angle that water exhibits with the molded sheet is representative of the contact angle that water exhibits with the fiber 10. A lower contact angle generally indicates that the fiber 10 has increased hydrophilicity. Water typically exhibits a contact angle with each of the plurality of fibers 10 of less than or equal to 90° according to modified ASTM C813-90 (2009).
  • water typically exhibits a contact angle with each of the plurality of fibers 10 of less than or equal to 85°, of less than or equal to 80°, of less than or equal to 75°, of less than or equal to 70°, or of less than or equal to 65°, each according to modified ASTM C813-90 (2009).
  • Ductility of the composite material may be determined by (1) forming a dogbone specimen of the composite material and (2) evaluating the dog bone specimen for ductility. Non-limiting examples of the composite material are evaluated for ductility below.
  • the present disclosure further provides a method of forming the composite material.
  • the method includes the step of combining the plastic component 12 and the surfactant 14 to form the plurality of fibers 10.
  • the plastic component 12 and the surfactant 14 may be combined by any method known in the art to form the plurality of fibers 10.
  • the plastic component 12 and the surfactant 14 may be blended dry, and then compounded by extrusion to form extrudates. These extrudates may then be extruded, spun, and then drawn to form the plurality of fibers 10.
  • the plastic component 12 and the surfactant 14 are combined to form a mixture prior to forming the plurality of fibers 10.
  • the mixture may be described as a masterbatch.
  • the plastic component 12 and the surfactant 14 may be combined by any method known in the art to form the mixture.
  • the plastic component 12 and the surfactant 14 may be combined in a mixing vessel and/or a blender, such as a Henschell mixer. If present, the additives may also be combined with the plastic component 12 and/or the surfactant 14 to form the mixture.
  • the plastic component 12, the surfactant 14, and, if present, the additives may be blended thoroughly such that the surfactant 14 and, if present, the additives, are approximately uniformly dispersed in the mixture with the plastic component 12.
  • the step of combining the plastic component 12 and the surfactant 14 to form the plurality of fibers 10 includes extruding the plastic component 12 and the surfactant 14 through a first extruder at a temperature of from 185° C to 215° C to form at least one strand.
  • the step of extruding the plastic component 12 and the surfactant 14 to form at least one strand may alternatively be described as compounding.
  • the plastic component 12 and the surfactant 14 may be extruded by any extrusion process known in the art, such as direct extrusion, indirect extrusion and/or hydrostatic extrusion.
  • extruding the plastic component 12 and the surfactant 14 to form at least one strand results in increased dispersion of the surfactant 14 in the fiber 10.
  • Increased dispersion of the surfactant 14 in the fiber 10 may increase adhesion of the fiber 10 to the cementitious composition.
  • the first extruder may be any extruder known in the art to form the at least one strand.
  • the first extruder may be further defined as a single screw extruder, twin screw, or multiscrew extruder.
  • the first extruder is further defined as a single screw extruder.
  • the first extruder is further defined as a twin screw extruder.
  • the first extruder may be further defined as a (fully) intermeshing extruder.
  • the first extruder may be further defined as a co -rotating extruder.
  • the first extruder may have a length to diameter ratio (L/D) of from 35 to 1 to 45 to 1 , alternatively, 36 to 1 to 44 to 1, 37 to 1 to 43 to 1 , 38 to 1 to 42 to 1 , or 39 to 1 to 41 to 1.
  • the first extruder may include a screw rotating at a speed of 140 to 160 revolutions per minute (RPM), alternatively, 145 to 155 RPM, 146 to 154 RPM, 147 to 153 RPM, 148 to 152 RPM, 149 to 151 RPM.
  • the screw of the first extruder may be primarily conveying the mixture.
  • the first extruder may be a Leistritz 27 mm co-rotating twin screw extruder.
  • the first extruder includes multiple heating zones, e.g. nine heating zones, with each heating zone at a temperature of from 185° C to 215° C.
  • the first extruder may operate at any temperature known in the art. More specifically, the plastic component 12 and the surfactant 14 may be extruded as a hot extrusion and/or a warm extrusion which may depend on the melt temperature of the plastic component 12 and/or the surfactant 14. It is also to be appreciated that the first extruder may have any number of heating zones such as 1, 2, 3, 4, 5, 6, 7, 8, 10, 1 1, 12, 13, 14, 15, etc. with each heating zone independently at a temperature of from 185° C to 215° C.
  • the step of combining the plastic component 12 and the surfactant 14 to form the plurality of fibers 10 includes quenching the at least one strand with water and subsequently cutting the at least one strand quenched with water to form pellets.
  • the at least one strand may be quenched in a water bath, by spray quenching, and/or by water wall quenching.
  • the at least one strand is quenched by air quenching to form pellets.
  • Cutting the at least one strand quenched with water (or by air quenching) may be performed by any cutting method known in the art such as with a ConAir pelletizer.
  • the pellets may have any dimensions and/or size distribution known in the art. In various embodiments, the pellets have a diameter of from 1/16 to 1/4 inch and a length of from 1/16 to 1/4 inch.
  • the step of combining the plastic component 12 and the surfactant 14 to form the plurality of fibers 10 includes extruding the pellets through a second extruder to form the plurality of fibers 10.
  • the second extruder may be any extruder known in the art to form the plurality of fibers 10.
  • the pellets may be extruded by extrusion spinning to form the plurality of fibers 10.
  • the plurality of fibers 10 may be cut such that each of the plurality of fibers 10 has a length of 1/4 to 3/4 inch.
  • the plurality of fibers 10 may be cut to a length of any size known in the art.
  • the method also includes the step of disposing the plurality of fibers 10 in the cementitious composition to form the composite material.
  • the plurality of fibers 10 may be disposed in the cementitious composition by any method know in the art. It is to be appreciated that the plurality of fibers 10 may be disposed in the aggregate, the binder, the water, cementitious materials, water reducers, air entrainers, accelerators, retarders, and/or fly ash prior to forming the cementitious composition so long as the plurality of fibers 10 is disposed in the cementitious composition.
  • Polypropylene, a surfactant, and additives are combined to form a mixture in a Henschell mixer.
  • the polypropylene is in solid form as a powder and formed from a nominal 12 melt polypropylene index homopolymer.
  • the mixture is blended thoroughly such that the surfactant and the additives are uniformly dispersed with the polypropylene.
  • the mixture is compounded in a Leistritz 27 mm co-rotating twin screw extruder (first extruder) to form at least one strand.
  • the first extruder is a co-rotating and fully intermeshing extruder.
  • the screw of the first extruder is primarily conveying and rotating at a speed of 150 RPM.
  • the first extruder has a L/D of 40 to 1.
  • the first extruder is equipped with a K-tron screw type feeder.
  • the first extruder has nine heating zones with each zone having a temperature profile as shown below. Zone #2: 190 °C
  • the mixture is heated in Zone #2 and Zone #4 and the die is heated in Zone #9.
  • the at least one strand is quenched in a water bath, and subsequently cut with a ConAir pelletizer to form pellets such that the pellets have a diameter of approximately 1/8 inch and a length of approximately 1/8 inch.
  • the pellets are extruded in a second extruder to form the plurality of fibers.
  • the plurality of fibers is cut to lengths of approximately 1/2 inch. Table I below illustrates formulas and results for water absorption for the plurality of fibers formed above.
  • a molded sheet is formed from the polypropylene and the surfactant to determine the contact angle that water exhibits with the molded sheet.
  • the contact angle that water exhibits with the molded sheet is representative of the contact angle that water exhibits with the fiber. Table I below also illustrates results for contact angle for the molded sheet described above.
  • Surfactant 1 (w/w) 1 — 3 —
  • Surfactant 2 (w/w) — 1 — —
  • Antioxidant w/w
  • Polypropylene is a polypropylene homopolymer commercially available from LyondellBasell Industries as Pro-faxTM 6301.
  • Surfactant 1 is an EO/PO block/heteric copolymer commercially available from BASF Corporation.
  • Surfactant 2 is another EO PO block/heteric copolymer commercially available from BASF Corporation.
  • HALS is a hindered amine light stabilizer commercially available from BASF Corporation as Chimassorb ® 2020.
  • Antioxidant is an antioxidant commercially available from BASF Corporation as Irganox ® B 1411 (AO).
  • the fibers of Examples 1 through 3 which include the surfactant have a greater water absorption than that of the fiber of the Comparative Example. As described above, a greater water absorption of the fibers generally indicates that the fibers have increased hydrophilicity. Moreover, Example 3 which has 3 parts by weight of Surfactant 1 , has an greater water absorption than that of Example 1 which has 1 part by weight of Surfactant 1. As such, the amount of surfactant in the fiber generally relates to water absorption of the fiber. Said differently, the greater the amount of surfactant in the fiber typically results in the greater the amount of water absorption of the fiber.
  • the molded sheets of Examples 1 through 3 which include the surfactants have a lower contact angle than that of the molded sheet of the Comparative Example.
  • a lower contact angle generally indicates that the fiber has increased hydrophilicity.
  • the increased hydrophilicity of the fiber generally indicates that the fiber has increased adhesion to the concrete.
  • Fibers of Examples 1 through 3 and the Comparative Example of Table I are each combined with concrete to each form a dogbone specimen of a composite material.
  • the dogbone specimen is formed by first casting the composite material including concrete and the fibers.
  • the dogbone specimen has an upper and lower end opposite to each other and a top and bottom surface extending along the dog bone specimen with the top and bottom surface opposite to each other.
  • the dogbone specimen is moisture cured for 7 days, and then air dried.
  • the top and bottom surfaces of the dogbone specimen are then leveled by a grinder.
  • the top and/or bottom surfaces are then marked 60 millimeters (mm) from each of the upper and lower ends.
  • the dogbone specimen is placed in an Instron test machine having a first and second clamp.
  • the first clamp applies 70 psi of pressure to the upper end of the dogbone specimen and the second clamp applies 70 psi of pressure to the lower end of the dogbone specimen to ensure that the dogbone specimen does not slip.
  • Load tension stress
  • Load is then applied to the dogbone specimen by the Instron test machine at a loading rate of 0.03 millimeters per minute (mm/min) until an extension (displacement) of 5 mm is achieved or the load drops by fifty percent of the peak load.
  • the tension stress over displacement is charted graphically.
  • the composite materials including the fiber of Examples 1 through 3 are evaluated for ductility against the composite material including the fibers of the Comparative Example. Table II below illustrates formulas for the composite materials and Figure 2 provides ductility represented by tensile stress versus displacement for the composite materials.
  • Concrete is a reaction product of binder, aggregate, and water with the binder present in an amount of 68 parts by weight, the aggregate present in an amount of 15 parts by weight, and the water present in an amount of 17 parts by weight.
  • the amount of tensile stress required to acheive a displacement of each of Examples 1 through 3 is significantly higher than the amount of tensile stress required to achieve a similar displacement of the Comparative Example.
  • This increased ductility of Examples 1 through 3 is most likely due to the increased adhesion the fibers of Examples 1 through 3 have to the concrete.
  • increasing the ductility of the composite material typically lowers the brittleness of the composite material such that the tensile strength of the composite material is increased.
  • any ranges and subranges relied upon in describing various embodiments of the present disclosure independently and collectively fall within the scope of the appended claims, and are understood to describe and contemplate all ranges including whole and/or fractional values therein, even if such values are not expressly written herein.
  • One of skill in the art readily recognizes that the enumerated ranges and subranges sufficiently describe and enable various embodiments of the present disclosure, and such ranges and subranges may be further delineated into relevant halves, thirds, quarters, fifths, and so on.
  • a range "of from 0.1 to 0.9" may be further delineated into a lower third, i.e., from 0.1 to 0.3, a middle third, i.e., from 0.4 to 0.6, and an upper third, i.e., from 0.7 to 0.9, which individually and collectively are within the scope of the appended claims, and may be relied upon individually and/or collectively and provide adequate support for specific embodiments within the scope of the appended claims.
  • a range of “at least 10” inherently includes a subrange of from at least 10 to 35, a subrange of from at least 10 to 25, a subrange of from 25 to 35, and so on, and each subrange may be relied upon individually and/or collectively and provides adequate support for specific embodiments within the scope of the appended claims.
  • an individual number within a disclosed range may be relied upon and provides adequate support for specific embodiments within the scope of the appended claims.
  • a range "of from 1 to 9" includes various individual integers, such as 3, as well as individual numbers including a decimal point (or fraction), such as 4.1 , which may be relied upon and provide adequate support for specific embodiments within the scope of the appended claims.

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Abstract

L'invention concerne un matériau composite comprenant une composition cimentaire renfermant plusieurs fibres. Chacune des fibres comprend un composant en matière plastique. Chacune des fibres comprend par ailleurs un tensioactif dispersé de manière hétérogène dans les fibres. Le tensioactif comprend un alcoxylat d'alcool, un alcoxylat d'alcool séquencé/hétérique, un copolymère polyoxyéthylène/polyoxypropylène séquencé/hétérique, un alcool gras, un alcool alcoxy gras, un polyalkylène glycol, un alcoxylat d'alkylphénol ou leurs associations. Le procédé de formation du matériau composite consiste à associer le composant en matière plastique et le tensioactif pour former les fibres. Le procédé consiste également à disposer lesdites fibres dans la composition cimentaire pour former le matériau composite.
PCT/EP2014/052283 2013-03-15 2014-02-06 Matériau composite contenant des fibres hydrophiles en matière plastique WO2014139734A1 (fr)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0240167A2 (fr) * 1986-03-03 1987-10-07 Exxon Chemical Patents Inc. Composition pour préparer des fibres renforçant le ciment
WO1994020654A1 (fr) * 1993-03-12 1994-09-15 Neste Oy Materiau fibreux a base de polyolefines
JP2002348157A (ja) * 2001-05-25 2002-12-04 Hagihara Industries Inc セメント強化用繊維
US20130048285A1 (en) * 2011-08-31 2013-02-28 Stephane Boulard Compositions and Methods for Servicing Subterranean Wells
WO2013166568A1 (fr) * 2012-05-07 2013-11-14 Braskem S.A. Procédé de granulation de polyoléfine, résine de polyoléfine, fibre de polyoléfine, utilisation de cette fibre de polyoléfine et composite cimentaire

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0240167A2 (fr) * 1986-03-03 1987-10-07 Exxon Chemical Patents Inc. Composition pour préparer des fibres renforçant le ciment
WO1994020654A1 (fr) * 1993-03-12 1994-09-15 Neste Oy Materiau fibreux a base de polyolefines
JP2002348157A (ja) * 2001-05-25 2002-12-04 Hagihara Industries Inc セメント強化用繊維
US20130048285A1 (en) * 2011-08-31 2013-02-28 Stephane Boulard Compositions and Methods for Servicing Subterranean Wells
WO2013166568A1 (fr) * 2012-05-07 2013-11-14 Braskem S.A. Procédé de granulation de polyoléfine, résine de polyoléfine, fibre de polyoléfine, utilisation de cette fibre de polyoléfine et composite cimentaire

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