WO1997012945A1 - Agents thixotropes aqueux pour systemes a base aqueuse - Google Patents
Agents thixotropes aqueux pour systemes a base aqueuse Download PDFInfo
- Publication number
- WO1997012945A1 WO1997012945A1 PCT/US1996/015940 US9615940W WO9712945A1 WO 1997012945 A1 WO1997012945 A1 WO 1997012945A1 US 9615940 W US9615940 W US 9615940W WO 9712945 A1 WO9712945 A1 WO 9712945A1
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- WO
- WIPO (PCT)
- Prior art keywords
- fumed silica
- waterborne
- sample
- aqueous
- dispersion
- Prior art date
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/04—Thixotropic paints
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B65—CONVEYING; PACKING; STORING; HANDLING THIN OR FILAMENTARY MATERIAL
- B65H—HANDLING THIN OR FILAMENTARY MATERIAL, e.g. SHEETS, WEBS, CABLES
- B65H2405/00—Parts for holding the handled material
- B65H2405/40—Holders, supports for rolls
- B65H2405/42—Supports for rolls fully removable from the handling machine
- B65H2405/422—Trolley, cart, i.e. support movable on floor
Definitions
- the present invention relates to aqueous thixotropes for waterborne systems and, more particularly, to aqueous dispersions of fumed silica for use as effective thixotropes and rheology control agents in waterborne systems.
- hydrophilic and hydrophobic fumed silicas are widely used in the coating industry to improve rheology, for flow control and storage stability, as well as serve as an anti-settling agent for pigments and fillers.
- the production of hydrophilic fumed silica is a well known process. Grades vary in particle and aggregate size.
- Hydrophobic silica can be produced by treating a fumed silica with a suitable agent which will vary depending on the desired degree of hydrophobicity and other characteristics.
- Such treating agents include, for example, polydimethylsiloxane oils of various molecular weights, dimethyldichlorosilane, trimethoxyoctylsilane, disilazanes, such as hexamethyldisilazane (HMDZ),and mixtures thereof.
- polydimethylsiloxane oils of various molecular weights dimethyldichlorosilane, trimethoxyoctylsilane, disilazanes, such as hexamethyldisilazane (HMDZ),and mixtures thereof.
- HMDZ hexamethyldisilazane
- untreated (hydrophilic) silicas are typically not effective because of the large concentrations of silica that are necessary to realize the desired thickening.
- the correct additive can often facilitate efficient viscosity and thixotropic control.
- the additives that are typically most useful in improving the thickening and thixotropic efficiency of fumed silica are cationic surfactants.
- the surfactants modify and partially impede the interaction between fumed silica and the solvent, thereby allowing the fumed silica network structure to develop, thus resulting in improved viscosity, thixotropy, and suspending properties.
- the additives which prove most useful are short chain molecules with more than one functional group capable of hydrogen bonding, such as glycols. These molecules act as bridging compounds between the surface hydroxyls of fumed silica aggregates, which form chains consisting of alternating silica aggregates and organic molecules. Such systems require the separate addition of certain additives to untreated silica dispersions.
- aqueous systems are increasingly used in many applications such as automotive and industrial coatings, paints, inks, adhesives, and the like.
- hydrophilic and hydrophobic silicas have both been used in solvent-based coating formulations on a commercial scale, their use in aqueous formulations have been plagued with disadvantages.
- either the silica additive must be increased to unacceptable levels or the formulation does not attain the desired level of performance.
- a demand therefore, exists for aqueous systems which perform comparably to solvent based systems and, accordingly, for improved additives or methods to accomplish such results.
- a further object is to provide an additive that fosters stability in aqueous compositions.
- a still further object is to provide a thixotrope which alleviates many of the waterborne coating rheology control formulating difficulties that exist with other inorganic and organic materials .
- the present invention is directed to an aqueous dispersion of fumed silica that provides enhanced rheology control and thixotropy to waterborne systems.
- the fumed silica dispersion is uniformly dispersed in the waterborne system such that an amount ranging between 0.5 % and 10.0 % , by weight, of silica is present in the final composition.
- the waterborne system therefore, includes an aqueous dispersion of fumed silica, and a waterborne resin.
- the resin is selected from the group consisting of alkyd, acrylic, polyester, polyether, silicate, urethane, epoxy, formaldehyde, vinyl, and mixtures thereof.
- the fumed silica has a surface area between about 85 m 2 /g and about 410 m 2 /g.
- FIG. 1 is a graph of the rheological performance of an epoxy resin system incorporating the present fumed silica dispersion
- FIG. 2 is a graph of the rheological performance of an bisphenol-A epoxy resin system incorporating the present fumed silica dispersion
- FIG. 3 is a graph of the rheological performance of an epichlorohydrin and bisphenol-A resin system inco ⁇ orating the present fumed silica dispersion
- FIG. 4 is a graph of the rheological performance of a urethane modified epoxy resin system inco ⁇ orating the present fumed silica dispersion
- FIG. 5 is a graph of the rheoiogical performance of an acrylic resin system inco ⁇ orating the present fumed silica dispersion
- FIG. 6 is a graph of the response of the present fumed silica dispersion in a typical water reducing alkyd coating formulation.
- the present invention is directed to an aqueous dispersion of hydrophilic fumed silica which provides enhanced rheology control and thixotropy to aqueous or waterborne systems.
- the present aqueous dispersion of fumed silica is effective in alkyd, acrylic, polyester, polyether, silicate, urethane, epoxy, formaldehyde, vinyl, and mixtures or modifications thereof as vehicle systems. It has been found that unlike other organic and inorganic materials used as thixotropes in waterborne systems such as coatings, the present aqueous dispersion of fumed silica will not typically react with additives in the formulation to produce unexpected side effects after product manufacture.
- Fumed silicas useful in this invention are generally characterized by a chain-like structure having high surface area per unit weight.
- the production of fumed silica is a well-documented process which involves the hydrolysis of silicon tetrachloride vapor in a flame of hydrogen and oxygen. Molten particles of roughly spherical shapes are formed in the combustion process, the diameters of which are varied through process parameters. These molten spheres of fumed silica, typically referred to as primary particles, fuse with one another by undergoing collisions at their contact points to form branched, three dimensional chain-like aggregates. The force necessary to break aggregates is considerable and often considered irreversible because of the fusion.
- agglomerates are thought to be loosely held together by Van der Waals forces and can be reversed, i.e. de-agglomerated, by proper dispersion in suitable media.
- the size of the primary spherical particles that comprise the fumed silica aggregates determine the surface area.
- the surface area of the fumed silica as measured by the nitrogen adso ⁇ tion method of S. Brunauer, P. H. Emmet, and I. Teller, J. Am. Chemical Society, Volume 60, Page 309 (1938) and commonly referred to as BET, typically ranges from about 85 m 2 /g to about 410 ⁇ r/g.
- the fumed silica is preferably in a range from about 175 m 2 /g to about 225 m 2 /g, and are of a high purity.
- High purity means that the total impurity content is typically less than 1 % and preferably less than 0.01 % (i.e., 100 ppm).
- fumed silicas are suitable, CAB-O-SIL ® fumed silica, available from the Cab-O-Sil Division of Cabot Co ⁇ oration, Tuscola, IL, having a surface area of about 200 m 2 /g is most preferred. Such a silica has been found to be of high quality and is readily dispersable.
- the fumed silica of the present invention is uniformly dispersed in a stable aqueous medium (e.g. deionized water) using conventional methods known to those skilled in the art.
- a stable aqueous medium e.g. deionized water
- uniformly dispersed is meant that the aggregates are isolated and well distributed throughout the medium.
- stable is typically meant that the aggregates will not re-agglomerate and settle out (e.g. form a hard, dense sediment).
- the fumed silica dispersion should have a pH between 5.0 and 10.5 and may be adjusted by the addition of a suitable base such as sodium hydroxide, potassium hydroxide, ammonia and the like.
- the fumed silica dispersion of the present invention has a pH ranging between 7.0 and 9.5.
- the fumed silica dispersion of the present invention is preferably prepared by the method described by Miller et al., in U.S. Patent No. 5,246,624, the disclosure of which is inco ⁇ orated herein in its entirety by reference. Although many commercially available fumed silica dispersions are suitable, CAB-O-SPERSE ® aqueous fumed silica dispersions, available from the Cab-O-Sil Division of Cabot Co ⁇ oration, Tuscola, IL, are most preferred.
- the waterborne systems of the present invention are prepared by combining or mixing the aqueous dispersions of fumed silica directly with a waterborne resin, such as an alkyd, acrylic, polyester, silicate, urethane, epoxy, and the like, or with a formulation containing a waterborne resin under low shear conditions (i.e., to prevent foaming) until a uniform homogeneous composition is obtained.
- a waterborne resin such as an alkyd, acrylic, polyester, silicate, urethane, epoxy, and the like
- a formulation containing a waterborne resin under low shear conditions (i.e., to prevent foaming) until a uniform homogeneous composition is obtained.
- the fumed silica dispersions range from about 10% to about 45 % solids, by weight; and, preferably, between 15% and 30% solids, by weight.
- a fumed silica dispersion of about 20 % solids, by weight has been found to maximize the loading level of silica while maintaining the colloidal stability
- aqueous dispersions of fumed silica of the present invention are useful in aqueous systems to provide effective rheological control (i.e., viscosity and thixotropy) for example, in industrial and automotive coating, adhesive, paint, and ink applications. It has been found that another advantage of using an aqueous dispersion of fumed silica in waterborne resin systems is to provide rheology and sag control, and anti-settling. It is also believed that a stable matrix is formed in waterborne formulations after the inco ⁇ oration of the fumed silica dispersion due to electrostatic interaction.
- the matrix disintegrates, thereby reducing viscosity and permitting near-Newtonian flow.
- the inorganic matrix reforms at a predictable rate to provide resistance to sagging and edge-pull during film coalescence and/or cure. This matrix remains unmodified through the many physical film changes during conversion from liquid to solid, thus providing a predictable application consistency.
- the aqueous dispersion of fumed silica has been found to be an effective suspension agent in some formulations due to its internally-generated structure.
- the product forms a matrix capable of stopping or significantly retarding undesirable striation and pigment settling, even in products containing powdered zinc or other unusually heavy pigments.
- dry hydrophilic fumed silica to waterborne systems has been found to be ineffective as a rheology control agent.
- the viscosity of the system will tend to continually increase over time, thereby not achieving stability.
- the dry silica is difficult to handle and disperse, and may tend to settle out at higher loading levels.
- the present dispersions will not migrate in wet or dry films and are unaffected by heat and atmospheric exposure in the dried/cured film.
- the dispersion is inherently non-yellowing and will not contribute to color changes or drift in either the wet or dry state.
- the present aqueous dispersions of fumed silica are biologically inactive and is not expected support microbial activity.
- aqueous dispersions of fumed silica used as aqueous thixotropes in water based systems are responsive to changes in pH, but have been found to be effective in the 7.0 to 9.5 pH range commonly used in products formulated for industrial and commercial use.
- the present dispersions have also been found to be effective in higher pH ranges, depending specifically upon the individual formulation.
- the aqueous dispersion of fumed silica of the present invention has been shown to be effective in many systems used in formulating waterborne products.
- aqueous colloidal dispersion of fumed silica which can be used as an aqueous thixotrope in the present invention, was prepared and evaluated as follows.
- a scaled-up volume of the dispersion of EXAMPLE I was prepared, using 2-amino-2- methyl-1 -propanol, available as AMP-95TM from Angus Chemical Company, Buffalo Grove, IL, as the base-stabilizer. Approximately 1283.80 grams of water were mixed with 0.251 gram of 38 % hydrochloric acid. About 499.92 grams of CAB-O-SIL ® PTG grade fumed silica were then added to the water/acid mixture, and was stirred for about 20 minutes. 678 grams of deionized water was then added to the mixture, followed by 10.54 grams of the AMP-95TM stabilizer. The aqueous fumed silica dispersion prepared had a 20.22% solids level, and a pH of 9.
- a waterborne system including an aqueous fumed silica dispersion (similar to the dispersion prepared in EXAMPLE I) and a waterborne epoxy resin, was prepared and evaluated to determine the effectiveness of the present dispersion as a thixotrope for waterborne systems.
- the aqueous fumed silica dispersion was mixed with Wate ⁇ oxy ® 701 Resin epoxy curing agent, available from Henkel Co ⁇ oration, Ambler, PA, until a loading level of 2% dry silica on resin solids was achieved.
- the viscosity (centipoise), shear thinning index (STI), and pH were then measured after sample preparation (0 days), and after periods of 1 and 7 days. The viscosity was measured on a Brookfield viscometer using Nos. 3 or 4 spindle at 6 and 60 RPM's. The experimental results are presented below in Table 1.
- FIG. 1 is a graph of the viscosity of a control sample (Sample 1), a waterborne epoxy resin without a rheology control agent, versus the present waterborne system (Sample 2) over time. Both Table 1 and FIG. 1 illustrate that the present waterborne system achieved stable performance after about 1 day and a desired increase in viscosity.
- a waterborne system including an aqueous fumed silica dispersion (similar to the dispersion prepared in EXAMPLE I) and a waterborne bisphenol-A epoxy resin, was prepared and evaluated to determine the effectiveness of the present dispersion as a thixotrope for waterborne systems.
- the aqueous fumed silica dispersion was mixed with EPI-REZ ® 3510-W-60 nonionic, aqueous dispersion of bisphenol-A epoxy resin, available from Shell Chemical Co. , Houston, TX, until a loading level of 2% dry silica on resin solids was achieved.
- the viscosity (centipoise), shear thinning index (STI), and pH were then measured after sample preparation (0 days), and after periods of 1 and 7 days.
- the viscosity was measured on a Brookfield viscometer using Nos. 3 or 4 spindle at 6 and 60 RPM's. The experimental results are presented below in Table 2.
- FIG. 2 is a graph of the viscosity of a control sample (Sample 1), a waterborne bisphenol-A epoxy resin without a rheology control agent, versus the present waterborne system
- Example 2 over time. Both Table 2 and FIG. 2 illustrate that the present waterborne system achieved stable performance, particularly the Sample 2 measured at 60 RPM, and a desired increase in viscosity. The Sample 2 viscosity measured at 6 RPM decreased more rapidly.
- a waterborne system including an aqueous fumed silica dispersion (similar to the dispersion prepared in EXAMPLE I) and a waterborne epichlorohydrin and bisphenol-A epoxy resin, was prepared and evaluated to determine the effectiveness of the present dispersion as a thixotrope for waterborne systems.
- the aqueous fumed silica dispersion was mixed with EPI- REZ ® 3510-WY-55 (55% solids) dispersion of EconTM 1001F condensation product of epichlorohydrin and bisphenol-A in water, available from Shell Chemical Co. , Houston, TX, until a loading level of 2% dry silica on resin solids was achieved.
- the viscosity (centipoise), shear thinning index (STI), and pH were then measured after sample preparation (0 days), and after periods of 1 and 7 days.
- the viscosity was measured on a Brookfield viscometer using Nos. 3 or 4 spindle at 6 and 60 RPM's. The experimental results are presented below in Table 3.
- FIG. 3 is a graph of the viscosity of a control sample (Sample 1), a waterborne epichlorohydrin and bisphenol-A epoxy resin without a rheology control agent, versus the present waterborne system (Sample 2) over time. Both Table 3 and FIG. 3 illustrate that the present waterborne system achieved a desired increase in viscosity while providing semi-stable performance in thixotropy.
- the Sample 2 viscosity measured 6 RPM increased rapidly.
- the Sample 2 measured at 60 RPM increased less rapidly and was more stable.
- a waterborne system including an aqueous fumed silica dispersion (similar to the dispersion prepared in EXAMPLE I) and a waterborne urethane modified epoxy resin, was prepared and evaluated to determine the effectiveness of the present dispersion as a thixotrope for waterborne systems.
- the aqueous fumed silica dispersion was mixed with EPI-REZ ® 5520- W-60 nonionic aqueous dispersion of urethane modified epoxy resin, available from Shell Chemical Co., Houston, TX, until a loading level of 2% dry silica on resin solids was achieved.
- the viscosity (centipoise), shear thinning index (STI), and pH were then measured after sample preparation (0 days), and after periods of 1 and 7 days.
- the viscosity was measured on a Brookfield viscometer using Nos. 3 or 4 spindle at 6 and 60 RPM's. The experimental results are presented below in Table 4.
- FIG. 4 is a graph of the viscosity of a control sample (Sample 1), a waterborne urethane modified epoxy resin without a rheology control agent, versus the present waterborne system (Sample 2) over time. Both Table 4 and FIG. 4 illustrate that the present waterborne system achieved stable performance after about 1 day and a desired increase in viscosity.
- a waterborne system including an aqueous fumed silica dispersion (similar to the dispersion prepared in EXAMPLE I) and a waterborne acrylic copolymer resin, was prepared and evaluated to determine the effectiveness of the present dispersion as a thixotrope for waterborne systems.
- the aqueous fumed silica dispersion was mixed with Neocryl ® A-639 waterborne acrylic copolymer, available from Zeneca Resins, Wilmington, MA, until a loading level of 2% dry silica on resin solids was achieved.
- the viscosity (centipoise), shear thinning index (STI), and pH were then measured after sample preparation (0 days), and after periods of 1 and 7 days. The viscosity was measured on a Brookfield viscometer using Nos. 3 or 4 spindle at 6 and 60 RPM's. The experimental results are presented below in Table 5.
- FIG. 5 is a graph of the viscosity of a control sample (Sample 1), a waterborne urethane modified epoxy resin without a rheology control agent, versus the present waterborne system (Sample 2) over time. Both Table 5 and FIG. 5 illustrate that the present waterborne system achieved stable performance after about 1 day and desired increase in viscosity.
- Example 7 a similar formulation utilizing an aqueous fumed silica dispersion (similar to the dispersion prepared in Example I) as an aqueous thixotrope (Sample).
- the viscosity of the coatings was measured on a Brookfield Rotary Viscometer RVD-II using spindle Nos. 1 or 2 at speeds of 0.5, 1.0, 2.5, 5.0, and 10.0 RPM.
- the STI is a ratio of the measured viscosity at 0.5 and 5.0 RPM's.
- Table 7 The experimental results are presented below in Table 7.
- the aqueous dispersion of the present invention can be inco ⁇ orated not only in resins but also in coating formulations.
- FIG. 6 is a graph illustrating the viscosity aging over time, taken from the data in Table 9, and corresponding to a shear rate of 1.4 dynes/sec.
- the aqueous dispersion of the present invention can be inco ⁇ orated not only in resins but also in coating formulations.
Abstract
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
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AU73902/96A AU7390296A (en) | 1995-10-06 | 1996-10-04 | Aqueous thixotropes for waterborne systems |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
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US540395P | 1995-10-06 | 1995-10-06 | |
US08/540,395 | 1995-10-06 |
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WO1997012945A1 true WO1997012945A1 (fr) | 1997-04-10 |
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PCT/US1996/015940 WO1997012945A1 (fr) | 1995-10-06 | 1996-10-04 | Agents thixotropes aqueux pour systemes a base aqueuse |
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AU (1) | AU7390296A (fr) |
WO (1) | WO1997012945A1 (fr) |
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