Source: http://www.google.com/patents/US8129018?dq=6322901
Timestamp: 2014-12-25 09:47:28
Document Index: 618123883

Matched Legal Cases: ['Application No. 05753082', 'Application No. 07751796', 'Application No. 08', 'Application No. 07', 'Application No. 2', 'Application No. 200580020171', 'Application No. 200580020171', 'Application No. 200580020171', 'Application No. 200580020171', 'Application No. 200780006861', 'Application No. 2007', 'Application No. 2006']

Patent US8129018 - Sizing for high performance glass fibers and composite materials ... - Google PatentsSearch Images Maps Play YouTube News Gmail Drive More »Sign inAdvanced Patent SearchPatentsA sizing composition containing an epoxy film former, a urethane film former, a silane package that includes an aminosilane coupling agent and an epoxy silane coupling agent, a cationic lubricant, a non-ionic lubricant, an antistatic agent, and at least one acid is provided. The epoxy resin emulsion...http://www.google.com/patents/US8129018?utm_source=gb-gplus-sharePatent US8129018 - Sizing for high performance glass fibers and composite materials incorporating sameAdvanced Patent SearchPublication numberUS8129018 B2Publication typeGrantApplication numberUS 11/362,987Publication dateMar 6, 2012Filing dateFeb 27, 2006Priority dateJun 18, 2004Also published asCA2641644A1, CN101553443A, EP1993966A2, EP1993966B1, US20060204763, WO2007100816A2, WO2007100816A3Publication number11362987, 362987, US 8129018 B2, US 8129018B2, US-B2-8129018, US8129018 B2, US8129018B2InventorsDavid R. Hartman, Luc M. Peters, Jeffrey L. AntleOriginal AssigneeOcv Intellectual Capital, LlcExport CitationBiBTeX, EndNote, RefManPatent Citations (50), Non-Patent Citations (30), Classifications (25), Legal Events (2) External Links: USPTO, USPTO Assignment, EspacenetSizing for high performance glass fibers and composite materials incorporating sameUS 8129018 B2Abstract A sizing composition containing an epoxy film former, a urethane film former, a silane package that includes an aminosilane coupling agent and an epoxy silane coupling agent, a cationic lubricant, a non-ionic lubricant, an antistatic agent, and at least one acid is provided. The epoxy resin emulsion includes a low molecular weight liquid epoxy resin and one or more surfactants. The epoxy resin preferably has an epoxy equivalent weight from 185-192. The sizing composition may optionally contain a methacryloxy silane. The sizing composition may be used to size glass fibers used in filament winding applications to form reinforced composite articles with improved mechanical properties, wet tensile properties, improved resistance to cracking, and improved processing characteristics.
Having thus described the invention, what is claimed is: 1. An aqueous sizing composition comprising:
CROSS REFERENCE TO RELATED APPLICATIONS This application is a continuation-in-part of U.S. patent application Ser. No. 11/197,864 entitled �Epoxy Sizing Composition for Filament Winding� filed Aug. 5, 2005 (now abandoned), which is a continuation-in-part of U.S. patent application Ser. No. 10/872,103 entitled �Epoxy Sizing Composition For Filament Winding� filed Jun. 18, 2004 (now U.S. Pat. No. 7,465,764) the entire contents of these applications is expressly incorporated herein by reference.
TECHNICAL FIELD AND INDUSTRIAL APPLICABILITY OF THE INVENTION The present invention relates generally to size compositions for glass fibers, and more particularly, to size compositions containing an epoxy emulsion and urethane for sizing glass fibers. The sized fibers are especially useful on fibers that will undergo a subsequent processing step such as knitting or weaving. The sized fibers especially suitable for use in reduced weight composite materials. Composite article including wind turbine blades and nacelles, aircraft interior and exterior parts, vehicle and infrastructure armor, transmission cable, automotive parts, high pressure tanks such as CNG/LNG tanks, high pressure pipe oil platform structures, electronic devices ceramic ware and heat resistant an filtration substrates formed from fibers sized with the sizing composition is also provided.
BACKGROUND OF THE INVENTION Glass fibers are useful in a variety of technologies. For example, glass fibers are commonly used as reinforcements in polymer matrices to form glass fiber reinforced plastics or composites because they provide dimensional stability as they do not shrink or stretch in response to changing atmospheric conditions. In addition, glass fibers have high tensile strength, heat resistance, moisture resistance, and low thermal conductivity.
Recently Owens Corning (of Toledo, Ohio, USA) has developed High Performance (HP) glass that may be inexpensively formed into glass fiber using low-cost, direct melting in refractory-lined furnaces due to the relatively low fiberizing temperature. These HP fibers are disclosed in U.S. patent application Ser. No. 11/267,702 entitled �Composition For High Performance Glass� filed Nov. 5, 2005, the entire content of which is expressly incorporated herein by reference. Once formed into fibers, the glass composition provides the strength characteristics of higher-priced S-Glass fibers. The composition of the present invention is 60.5-70.5 weight % SiO2, 10.0-24.5 weight % Al2O3, 6.0 to 20.0 weight % RO where RO equals the sum of MgO, CaO, SrO and BaO, and 0.0 to 3.0 weight % alkali metal oxides. In a preferred embodiment, the glass composition is substantially 61-68 weight % SiO2, 15-19 weight % Al2O3, 15-20 weight % RO, 0 to 3 weight % ZrO2, and 0 to 3 weight % alkali metal oxides.
SUMMARY OF THE INVENTION It is an object of the present invention to provide a sizing composition for glass fibers that includes an epoxy resin emulsion, a urethane, a silane package that includes at least one aminosilane coupling agent and at least one epoxy silane coupling agent, a non-ionic lubricant, a cationic lubricant, an antistatic agent, an organic acid, and a boron-containing compound. The epoxy resin emulsion contains an epoxy resin and at least one surfactant. It is preferred that the epoxy resin have an epoxy equivalent weight from 180-210, and even more preferably from 180-195. Although the size composition may be applied to any glass fiber, the performance of the size is optimized when low-to-no boron-containing glass fibers are utilized.
BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1 is a bar chart showing testing for equal variances for flexural strength.
DETAILED DESCRIPTION AND PREFERRED EMBODIMENTS OF THE INVENTION Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which the invention belongs. Although any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present invention, the preferred methods and materials are described herein. All references cited herein, including published or corresponding U.S. or foreign patent applications, issued U.S. or foreign patents, or any other references, are each incorporated by reference in their entireties, including all data, tables, figures, and text presented in the cited references. It is to be noted that the phrases �size composition�, �sizing composition�, �size�, and �sizing� are used interchangeably herein.
The epoxy film forming polymer component of the sizing composition includes epoxy resin emulsions that contain a low molecular weight epoxy resin and at least one surfactant. The film former functions to protect the fibers from damage during processing and imparts compatibility of the fibers with the matrix resin. It is preferred that the epoxy resin have a molecular weight from 360-420 and an epoxy equivalent weight from 180-210, more preferably a molecular weight 360-390 and an epoxy equivalent weight from 180-195, and most preferably a molecular weight of 370-384 and an epoxy equivalent weight from 185-192. �Epoxy equivalent weight�, as used herein, is defined by the molecular weight of the epoxy resin divided by the number of epoxy groups present in the compound. Useful epoxy resins contain at least one epoxy or oxirane group in the molecule, such as polyglycidyl ethers of polyhydric alcohols or thiols. Examples of suitable epoxy film forming resins include Epon� 828 (available from Hexion Specialties Chemicals Incorporated), DER 331 (available from Dow Chemicals), Araldite 6010 (available from Huntsman), and Epotuf 37-140 (available from Reichhold Chemical Co).
The low molecular weight epoxy resin emulsions are in a liquid form which reduces, and in some cases, eliminates the need for a solvent such as diacetone alcohol. This reduction of organic solvents in turn reduces the amount of VOC's (volatile organic compounds) that are emitted into the working environment. In addition, the low molecular weight epoxy film forming emulsions according to the present invention are substantially color free. As used herein, the term �substantially color free� means that there is minimal or no coloration of the epoxy emulsions. Another advantage of the inventive epoxy emulsions is that they disperse easily in water. The inventive epoxy resins also provide for better wetting of the resin, a greater epoxy reactivity, improved coating quality, improved emulsion dispersion, and reduced strand stiffness.
55.8% 25-2828
32.9% EE732
Epirez 3511
64.1% W60
0.64% 1.2%
14.0% Z6026
Emerstat
100.00% 100.00% 100.00% 100%
100% TABLE 2
Stength 65%
The HP glasses are made from a range of glass compositions, as shown in the examples listed in Tables 9A-9C, which were melted in platinum crucibles or in a continuous platinum-lined melter for the purpose of determining the mechanical and physical properties of the glass and fibers produced therefrom. The fibers used to generate the data of Table 1-8 are shown in EX. 14. The units of measurement for the physical properties are: Viscosity (� F.), Liquidus temperature (� F.) and ΔT (� F.). In some examples the glasses were fiberized and Strength (KPsi), Density (g/cc), Modulus (MPsi), Softening Point (� F.) and coefficient of thermal expansion (CTE) (in/in/(� F.)) were measured.
Measured Viscosity (� F.)
Measured DT (� F.)
Measured Density (g/cc)
Additionally, the sizing composition contains at least one non-ionic lubricant. The non-ionic lubricant in the sizing composition acts as a �wet lubricant� and provides additional protection to the fibers during the filament winding process. In addition, the non-ionic lubricant helps to reduce the occurrence of fuzz. Especially suitable examples of non-ionic lubricants include PEG 200 Monolaurate (a polyethylene glycol fatty acid ester commercially available from Cognis) and PEG 600 Monooleate (Cognis). Other non-limiting examples include a polyalkylene glycol fatty acid such as PEG 600 Monostearate (a polyethylene glycol monostearate available from Cognis), PEG 400 Monostearate (Cognis), PEG 400 Monooleate (Cognis), and PEG 600 Monolaurate (Cognis). In a most preferred embodiment, the non-ionic lubricant is PEG 200 Monolaurate. The non-ionic lubricant may be present in the size composition in an amount from approximately 6-10% by weight solids, preferably from 7-9% by weight solids.
In addition to the non-ionic lubricant, the sizing composition also contains at least one cationic lubricant and at least one antistatic agent. The cationic lubricant aids in the reduction of interfilament abrasion. Suitable examples of cationic lubricants include, but are not limited to, a polyethyleneimine polyamide salt commercially available from Cognis under the trade name Emery 6760L, a stearic ethanolamide such as Lubesize K-12 (AOC), Cirrasol 185AE (Unichemie), and Cirrasol 185AN (Unichemie). The amount of cationic lubricant present in the size composition is preferably an amount sufficient to provide a level of the active lubricant that will form a coating with low fuzz development. In at least one exemplary embodiment, the cationic lubricant is present in the size composition in an amount from 0.01-1.0% by weight solids, preferably from 0.03-0.06% by weight solids. Antistatic agents especially suitable for use herein include antistatic agents that are soluble in the sizing composition. Examples of suitable antistatic agents include compounds such as Emerstat� 6660A and Emerstat� 6665 (quaternary ammonium antistatic agents available from Emery Industries, Inc.), and Larostat 264A (a quaternary ammonium antistatic agent available from BASF), tetraethylammonium chloride, and lithium chloride. Antistatic agents may be present in the size composition in an amount from 0.4-0.8% by weight solids, preferably from 0.4-0.6% by weight solids.
EPI-REZ Resin 3510-W-60, an aqueous dispersion of a low molecular weight liquid Bisphenol A epoxy resin (EPON� Resin 828-type); EPI-REZ Resin 3515-W-60, an aqueous dispersion of a semi-solid Bisphenol A epoxy resin; EPI-REZ Resin 3519-W-50, an aqueous dispersion of a CTBN (butadiene-acrylonitrile) modified epoxy resin; EPI-REZ Resin 3520-WY-55, an aqueous dispersion of a semi-solid Bisphenol A epoxy resin (EPON 1001-type) with an organic co-solvent; EPI-REZ Resin 3521-WY-53, a lower viscosity version of the EPI-REZ Resin 3520-WY-55 dispersion; EPI-REZ Resin 3522-W-60, an aqueous dispersion of a solid Bisphenol A epoxy resin (EPON 1002-type); EPI-REZ Resin 3535-WY-50; an aqueous dispersion of a solid Bisphenol A epoxy resin (EPON 1004-type) with an organic co-solvent; EPI-REZ Resin 3540-WY-55, an aqueous dispersion of a solid Bisphenol A epoxy resin (EPON 1007-type) with an organic co-solvent; EPI-REZ Resin 3546-WH-53, an aqueous dispersion of a solid Bisphenol A epoxy resin (EPON 1007-type) with a non HAPS co-solvent; EPI-REZ Resin 5003-W-55, an aqueous dispersion of an epoxidized Bisphenol A novolac resin with an average functionality of 3 (EPON SU-3 type); EPI-REZ Resin 5520-W-60, an aqueous dispersion of a urethane-modified Bisphenol A epoxy resin; EPI-REZ Resin 5522-WY-55, an aqueous dispersion of a modified Bisphenol A epoxy resin (EPON 1002-type) with an organic co-solvent; EPI-REZ Resin 6006-W-70, an aqueous dispersion of a epoxidized o-cresylic novolac resin with an average functionality of 6, each of which is commercially available from Resolution Performance Products.
The polyurethane film former increases strand integrity and the mechanical fatigue performance by toughening the resin/size interphase. The toughened resin interphase results in a final composite product that has an improved resistance to cracking and has increased or improved mechanical properties such as improved strength. The urethane film former may be present in the sizing composition an amount from about 2 to about 10% by weight solids, preferably in an amount from 2.5-7.5% by weight solids and most preferably of about 5.1% by weight solids. Suitable polyurethane dispersions include polyurethane emulsions such as Hydrosize� U1-01, U1-03, U2-01, U4-01, U5-01, U6-01, U6-03 and U7-01 available from Hydrosize� Technologies, Inc (Raleigh, N.C., USA)
Epoxy Resin Emulsion
Urethane Film Former
Non-Ionic Lubricant
Cationic Lubricant/Antistatic Agent
The size composition may be applied to strands of glass formed by conventional techniques such as by drawing molten glass through a heated bushing to form substantially continuous glass fibers. Any type of glass, such as A-type glass, C-type glass, E-type glass, S-type glass, R-type glass, AR-type glass, E-CR-type glass (commercially available from Owens Corning Fiberglass Corporation under the trade name Advantex�), or modifications thereof may be used. Although any glass fiber may be utilized, the size performance is optimized when High Performance (HP) glass fibers are used. The size composition may be applied to fibers having a diameter from about 5 to about 30 microns, with fibers from about 9 to about 30 microns in diameter being more preferred. For use in wind blade applications, the preferred diameter is between about 12 and 19 microns and 400 to 8000 tex. In addition, the size composition may be applied to single or multi-filament fiber strands. Each strand may contain from approximately 2000-4000 fibers.
EXAMPLES Rods were pultruded with epoxy MGS LI 35i resin (+137i hardener) and with Polyester Reichhold 513-575 (limited distribution to LM) and with Advantex and HP-glass, 17-1200 tex rovings. The rods were submitted to 3-point bending tests and Short Beam Shear Strength (SBSS) tests following ISO 3597-2 and ISO 3597-4 respectively.
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No. 11/197,864 dated Oct. 8, 2008.Classifications U.S. Classification428/391, 252/8.83, 428/375International ClassificationB32B17/04, D06M15/55, D06M15/564, D06M13/50Cooperative ClassificationB29K2105/06, C03C3/087, C03C13/00, C03C25/26, C03C25/326, C03C25/36, C03C25/40, C08G59/245, C08G59/621, C08L63/00, C08L75/04European ClassificationC03C25/40, C03C25/26, C08L63/00, C08G59/24B, C03C25/32H, C08G59/62B, C03C25/36Legal EventsDateCodeEventDescriptionJun 11, 2009ASAssignmentOwner name: OCV INTELLECTUAL CAPITAL, LLC, OHIOFree format text: ASSIGNMENT OF ASSIGNORS INTEREST;ASSIGNOR:OWENS-CORNING FIBERGLAS TECHNOLOGY, INC.;REEL/FRAME:022804/0882Effective date: 20081121Owner name: OCV INTELLECTUAL CAPITAL, LLC,OHIOFree format text: ASSIGNMENT OF ASSIGNORS INTEREST;ASSIGNOR:OWENS-CORNING FIBERGLAS TECHNOLOGY, INC.;REEL/FRAME:22804/882Aug 4, 2006ASAssignmentOwner name: OWENS CORNING COMPOSITES SPRL, BELGIUMOwner name: OWENS-CORNING FIBERGLAS TECHNOLOGY, INC., ILLINOISFree format text: ASSIGNMENT OF ASSIGNORS INTEREST;ASSIGNORS:HARTMAN, DAVID R.;PETERS, LUC M.;ANTLE, JEFFREY L.;REEL/FRAME:018155/0267;SIGNING DATES FROM 20060406 TO 20060514Free format text: ASSIGNMENT OF ASSIGNORS INTEREST;ASSIGNORS:HARTMAN, DAVID R.;PETERS, LUC M.;ANTLE, JEFFREY L.;SIGNING DATES FROM 20060406 TO 20060514;REEL/FRAME:018155/0267RotateOriginal ImageGoogle Home - Sitemap - USPTO Bulk Downloads - Privacy Policy - Terms of Service - About Google Patents - Send FeedbackData provided by IFI CLAIMS Patent Services©2012 Google