COMPOSITION FOR ENHANCING THE PROPERTIES OF A SUBSTRATE AND METHOD FOR MAKING THE SAME

Abstract

A surface treatment composition including polymeric complex nanoparticles used in a hydrophobic agent and siloxane complex nanoparticles used in a suspending agent thereof. The composition of the present invention is a solution comprising a plurality of components. The primary components are an acid mixture and a base mixture that are combined together in a manner to be described herein to produce a two-part liquid solution. The two parts, are combined together prior to application to a surface and allowed to cure on the surface.

Claims

1. A composition for protecting a surface of a substrate, the composition comprising a mixture of: a. an Acid Mixture component including MKP (about 48% to about 72%), TiO.sub.2 (about 0.4% to about 4.8%), SiO.sub.2(about 0.6% to about 4.3%), K.sub.3PO.sub.4 (about 4.5% to about 13.5%), Hydrogen Hydroxide (about 18% to about 39%) and a hydrophobic agent (about 0.5% to about 20%); and b. a Base Mixture component including MgOH (about 28% to about 52%), Metakaolin (about 12% to about 31%), CaSiO3 (about 14% to about 33%), Siloxane (about 0.4% to about 3.6%), K.sub.3PO.sub.4 (about 1.2% to about 4.2%), Hydrogen Hydroxide (about 24% to about 48%) and a suspending agent (about 0.5% to about 20%).

2. The composition as claimed in claim 1 wherein the hydrophobic agent is a Nano Siloxane Complex comprising nanoparticles thereof.

3. The composition as claimed in claim 2 wherein the hydrophobic agent is selected from the group consisting of: Isobutyltrimethoxyisosilane, Isobutyltriethoxyisosilane, Triisobutylsilicateisosilane, Organofunctional Isobutyltrimethoxyisosilane, Organofunctional Isobutyltrimethoxyisosilane Hydroxy, Alkoxytrisilicateisobutylisosilane, Organofunctionallsobutyltrimethoxyisosilane Hydroxy, Alkoxytrisilicate Organofunctional Isobutyltrimethoxyisosilane Hydroxy, Triethoxymethylpropanalcyclicsilane, Alkoxytrisilicate, Organofunctional Isobutyltrimethoxyisosilane Hydroxy and Ethyltrichlorosilane carbomethoxy.

4. The composition as claimed in claim 2 wherein the hydrophobic agent nanoparticles are in the size range of about 15 nanometers to about 50 nanometers.

5. The composition as claimed in claim 1 wherein the suspending agent is a Nano Polymer Complex comprising nanoparticles thereof.

6. The composition as claimed in claim 5 wherein the suspending agent is selected from the group consisting of: Polyvinyl polymeric chloride, Vinyl chloride polymer, Polyvinyl alcohol, Cellulose ether copolymer, Mono diglyceride polymer, Polyvinyl acrylic resin, Styrene monomers, Acrylic monomer, and Vinyl acrylic polymer.

7. The composition as claimed in claim 5 wherein the suspending agent nanoparticles are in the size range of about 15 nanometers to about 50 nanometers.

8. The composition as claimed in claim 1 further comprising one or more additives.

9. The composition as claimed in claim 8 wherein the one or more additives are added to either or both of the Acid Mixture and the Base Mixture.

10. The composition as claimed in claim 8 wherein the one or more additives are selected from the group consisting of fiberglass, basalt and Aluminum.

11. A method of making a composition for protecting a surface of a substrate, the method comprising the steps of: a. creating an Acid Mixture component including MKP (about 48% to about 72%), TiO.sub.2(about 0.4% to about 4.8%), SiO.sub.2(about 0.6% to about 4.3%), K.sub.3PO.sub.4 (about 4.5% to about 13.5%), Hydrogen Hydroxide (about 18% to about 39%) and a hydrophobic agent (about 0.5% to about 20%); b. creating a Base Mixture component including MgOH (about 28% to about 52%), Metakaolin (about 12% to about 31%), CaSiO.sub.3 (about 14% to about 33%), Siloxane (about 0.4% to about 3.6%), K.sub.3PO.sub.4 (about 1.2% to about 4.2%), Hydrogen Hydroxide (about 24% to about 48%) and a suspending agent (about 0.5% to about 20%); and c. combining together the Acid Mixture and the Base Mixture.

12. The method as claimed in claim 11 wherein the step of combining includes the steps of stirring the Acid Mixture component and the Base Mixture component separately and then mixing the Acid Mixture and the Base Mixture together in a ratio of about 1:1.

13. A method of treating a surface of a substrate comprising the steps of: a. cleaning the surface so as to eliminate the existence of corroded material thereon; b. applying to the cleaned surface a first layer of a composition that includes a combination of an Acid Mixture and a Base Mixture; and c. applying to the first layer of the composition a second layer of the composition, wherein the Acid Mixture component includes MKP (about 48% to about 72%), TiO.sub.2(about 0.4% to about 4.8%), SiO.sub.2(about 0.6% to about 4.3%), K.sub.3PO.sub.4 (about 4.5% to about 13.5%), Hydrogen Hydroxide (about 18% to about 39%) and a hydrophobic agent (about 0.5% to about 20%), and the Base Mixture component includes MgOH (about 28% to about 52%), Metakaolin (about 12% to about 31%), CaSiO.sub.3 (about 14% to about 33%), Siloxane (about 0.4% to about 3.6%), K.sub.3PO.sub.4 (about 1.2% to about 4.2%), Hydrogen Hydroxide (about 24% to about 48%) and a suspending agent (about 0.5% to about 20%).

14. The method as claimed in claim 13 wherein the hydrophobic agent is a Nano Siloxane Complex comprising nanoparticles thereof.

15. The method as claimed in claim 13 wherein the suspending agent is a Nano Polymer Complex comprising nanoparticles thereof.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0015] A composition of the present invention for coating the surface of a substrate to protect that substrate from environmental conditions includes an Acid Mixture component, sometimes referred to herein as the Part A component, and a Base Mixture component, sometimes referred to herein as the Part B component.

[0016] Acid Mix. The Acid Mixture component is formed of the following components: Monopotassium Phosphate (MKP), Titanium Dioxide (TiO.sub.2), Hydrogen Hydroxide (H.sub.2O or water), Silicon Dioxide (SiO.sub.2), Tripotassium Phosphate, also referred to as Potassium Phosphate Tribasic (K.sub.3PO.sub.4), Phosphoric Acid and a hydrophobic agent. The hydrophobic agent may be a Nano Siloxane Complex comprising nano particles in the size range of about 20 nanometers (nm) to about 50 nm. The hydrophobic agent may be selected from the group consisting of: Isobutyltrimethoxyisosilane, Isobutyltriethoxyisosilane, Triisobutylsilicateisosilane, Organofunctional Isobutyltrimethoxyisosilane, Organofunctional Isobutyltrimethoxyisosilane Hydroxy in cap; Alkoxytrisilicateisobutylisosilane, Organofunctionallsobutyltrimethoxyisosilane Hydroxy in cap; Alkoxytrisilicate Organofunctional Isobutyltrimethoxyisosilane Hydroxy in cap; Triethoxymethylpropanalcyclicsilane, Alkoxytrisilicate; Organofunctional Isobutyltrimethoxyisosilane Hydroxy in cap OH Reactive; and Ethyltrichlorosilane carbomethoxy. It is to be understood by those skilled in the art that “in cap” refers to hydroxyalkyl functional fluid polymerization that involves hydrolysable end caps, such as methoxy groups, wherein alkyl group components react with hydroxyl group components, resulting in end caps with methoxy groups.

[0017] Base Mix. The Base Mixture component is formed of the following components: Magnesium Hydroxide (MgOH), A pozzolon material that is a silicate material used to enhance the physical properties of a cementitious material, the pozzolon selected from the group consisting of Metakaolin, which is a dehydroxylated form of the clay mineral kaolinite, Calcium Silicate (CaSiO.sub.3), Aluminum Silicate (AlSiO.sub.3) and Fly Ash; Nano Siloxane Complex, K.sub.3PO.sub.4, Hydrogen Hydroxide and a suspending agent. The suspending agent may be a Nano Polymer Complex comprising nano particles in the size range of about 15 nm to about 50 nm. The suspending agent may be selected from the group consisting of Polyvinyl polymeric chloride; Vinyl chloride polymer; Polyvinyl alcohol; Cellulose ether copolymer; Mono diglyceride polymer; Polyvinyl acrylic resin; Styrene monomers; Acrylic monomer; and Vinyl acrylic polymer.

[0018] The listed components make up the composition in the following ranges of proportions by volume: [0019] Acid Mix=MKP (about 48% to about 72%), TiO.sub.2(about 0.4% to about 4.8%), SiO.sub.2 (about 0.6% to about 4.3%), K.sub.3PO.sub.4 (about 4.5% to about 13.5%), Hydrogen Hydroxide (about 18% to about 39%) and hydrophobic agent (about 0.5% to about 20%). [0020] Base Mix=MgOH (about 28% to about 52%), Pozzalon (about 12% to about 31%), CaSiO3 (about 14% to about 33%), Siloxane (about 0.4% to about 3.6%), K.sub.3PO.sub.4 (about 1.2% to about 4.2%), Hydrogen Hydroxide (about 24% to about 48%) and suspending agent (about 0.5% to about 20%).

[0021] The composition has been the subject of preliminary testing. The versions of the composition considered most promising include the following components in the indicated proportions by volume: PART-A: Water (H.sub.2O): about 25% to 35%, MKP: about 60% to 65%, Phosphoric Acid: about 6% to 10%, a water soluble polymer such as cellulose ether, which is available from the Dow Chemical Company under the trade name Methocel™: 0.12% to 0.18%, SiO.sub.2 1% to 5%, TiO.sub.2 1% to 4%, Nano Polymer Complex-1% to 8% and Nano Siloxane Complex 1% to 8%. PART-B: Hydrogen Hydroxide: about 30% to about 40%, K.sub.3PO.sub.4: about 2% to about 8%, Cellulose ether: about 0.12% to about 0.18%, Metakaolin that has been pozzolanized; that is, enhanced to improve the characteristics of a cementitious material, with the suspending agent): about 18% to about 26%, MgOH: about 38% to about 44% and an alkyphenol such as Nonylphenol: about 0.01% to about 0.05%. One or more additives including, but not limited to, fiberglass, basalt and/or Aluminum, may be added to either or both of Part A or Part B of the composition to enhance bonding, crosslinking and/or to increase flexural strength of the composition. Such additives may be in a relatively small physical form such as in the form of microfibers or microparticles, for example.

[0022] Different variations of the inventive composition can be made by changing proportions of the listed components but the process of combining them is generally the same for those variations. The primary common steps of the composition fabrication process include:

Part-A Mix:

[0023] 1—Mix the cellulose ether with Hydrogen Hydroxide for 10 to 12 minutes at room temperature. [0024] Allow that mixture to rest for 10 to 12 minutes and then check viscosity (Ford cup), maintaining between 18 to 20 seconds. [0025] 2—Add Phosphoric Acid to the above mix. Mix for 10 to 12 minutes. [0026] 3—Add SiO.sub.2 to the above mix. Mix for 5 to 7 minutes. [0027] 4—Add MgOH to the above mix. Mix for 5 to 7 minutes. [0028] 5—While mixing the mixture of step 4 above, add TiO.sub.2. [0029] 6—Continue to mix and add Nano Polymer Complex. [0030] 7—Continue to mix and add Nano Siloxane Complex. [0031] 8—Continue mix for 10 to 12 minutes until the mixture becomes a creamy stable suspension. [0032] 9—Let the above mix stand for one hour and or let it cool to room temperature. [0033] 10—Optionally, retain batch sample.

Part-B Mix:

[0034] 1—Mix K.sub.3PO.sub.4, with Hydrogen Hydroxide for 5 to 7 minutes. Let mix temperature drop back to 75 F to 80 F. [0035] 2—Continue to mix and add cellulose ether. Mix for 10 minutes. Let this mix rest for 10 minutes and then check viscosity (Ford cup), maintaining between 8 to 11 seconds. [0036] 3—While mixing the mixture of step 2 above, add pozzolanized Metakaolin. Mix for 5 minutes. [0037] 4—Start mixing and add MgOH. Mix for 10 minutes and allow that mixture to rest for 10 minutes. Maintain temperature below or less than 110 F to 115 F. Do not let this mix temperature climb over 120 F. Let this mix temperature cool down to less than 80 F. [0038] 5—While mixing the mixture of step 4 above, add alkylphenol. Mix for 5 minutes. Let mix set for one hour before filling containers. [0039] 6—Optionally, retain batch sample.

[0040] In all instances, proper quality control is maintained. For example, but not limited, all component amounts should be measured with suitable accuracy, contaminants are to be avoided, all components must be properly stored. All components should be premeasured, whether by weight or volume prior to mixing. All mixing must be done thoroughly and may be done with mechanical mixing, such as with a Hobart mixer, for example. Cross contamination and foreign particulate are to be avoided.

[0041] The mix ratio of Part A and Part B to form the composition of the present invention is about 1:1. When a user is ready to apply the composition to a substrate, Part A and Part B are individually stirred for at least three minutes and then mixed together at a ratio of about 1:1 ratio. The composition is initially provided in liquid form that is applied, such as by spraying, to the surface of a substrate to be protected. The surface must be as clean as possible without corroded material thereon. The sprayed composition initially forms a transparent layer that turns opaque upon curing. The composition is applied in at least two steps. A first layer is applied as a thin film that bonds to the surface of the substrate by integrating with microscopic interstices on the surface. The second layer is applied to and bonds to the first layer and is exposed to the atmosphere. The combination of layers thereby protects the substrate. The composition is not applied or used so as to be removed from the surface of the substrate.

[0042] Versions of the composition of the present invention were prepared and evaluated for usability and functionality as a protective coating for a surface. Samples of two examples of the composition were analyzed for handling, sprayability and response to test environments in testing performed by the independent Constructed Facilities Laboratory at North Carolina State University. The samples were applied to sandblasted mild steel plates by the laboratory for evaluation. White blasted 4″×4″ steel plates were used as well as commercial blasted 3″×5″ plates. The samples consisted of a “Part A” and a “Part B” that were mixed, evaluated, and sprayed on steel plates using a hand-held cartridge sprayer with static mixing nozzle. In general, the samples sprayed well, flowing through the nozzle without clogging and allowed for a thin-film coating to be deposited on the steel surface. The examples of the coating composition examined formed a hard surface within minutes of spraying. Prior to spraying, the samples were reacted (Part A mixed with Part B) in a small cup, and all hardened in less than 2 minutes with mixing. Certain samples did have notable deficiencies in spraying, however, no deficiencies were significant enough to prevent application or to render an application unusable.

[0043] In addition to spraying steel samples, a large-scale demonstration was conducted. A rusted steel beam having dimensions of approximately 14″×30″×16′ was sandblasted to a commercial-grade finish. The beam was blown off with compressed air and was then sprayed with a thin coat of the samples. After coating the beam with a sample of the composition, the beam was then top-coated with a single layer of red enamel paint. A single layer of red topcoat was used, and during top coating, it was observed that the red paint covered the ceramic more easily than it covered bare steel. A single coat of red topcoat was used.

[0044] Salt tank drip testing was conducted on the samples. It was used to quickly evaluate the effectiveness of the coating of the present invention at protecting steel from corrosion. One coated steel plate from each sample was subjected to an intermittent stream of 5% Sodium Chloride (NaCl) solution (by mass). The intermittent stream was set on a timer to cycle 30 minutes on then 30 minutes off. Samples were compared visually before and after testing. Each sample was left in the test tank until substantial rusting of the steel sample was observed. All tested coupons were scratched to bare steel prior to testing in accordance with ASTM D1654. The specimens were angled at approximately 200 from the horizontal on a PVC support, allowing the stream of water to run down the scribe line of each specimen and flow off the bottom. The test was conducted in ambient laboratory conditions at a nominal temperature of 73° F. Tap water was added to the tank as needed to offset evaporation and to maintain a constant water level. Images were taken of each set of specimens at regular intervals. Prior to photographing, specimens were removed from the tank and rinsed with fresh water to remove surface debris and salt deposits. The plate coated with the composition of Example 1 described herein exhibited substantial rusting after 30 days. The plate coated with the composition of Example 2 described herein exhibited little rusting after 45 days.

[0045] Temperature resistivity of samples of coatings of the present invention were conducted to evaluate the ability of the coatings to sustain temperatures other than ambient. A 3×5 in. steel coupon was coated with the composition of Example 1 and was then placed in an oven at a constant temperature of 250° F. for 100 days. At the conclusion of the test, some surface map cracking was observed, but the ceramic coating remained visibly intact. A 3×5 in. steel coupon was also coated with the same composition, saturated with tap water and then placed in a freezer at 0° F. for 100 days. After 100 days, the coating remained well-bonded to the steel substrate, with a series of dark spots observed around the perimeter of the coupon. In addition, a 3×5 in. steel coupon that was coated with the composition of Example 1 was placed into a kiln for 19 days. The temperature in the kiln was gradually changed as follows: 350° F. for 5 days; then 550° F. for 7 days; then 650° F. for 2 days; then 750° F. for 1 day; then 850° F. for 2 days; then 1000° F. for 1 day. The kiln was then shut off and allowed to cool back to ambient temperature over the period of 1 day. After this process, the coupon was scribed in accordance with ASTM D1654 and placed in the salt dripping tank described above. It was observed that map cracking appeared at 350° F., a brownish color developed beyond 350° F., and the brownish color darkened as the test progressed.

[0046] Upon removal from the kiln, a coating was still present on the steel surface, however, it was significantly (but consistently) spotty in appearance. The kiln specimen was scribed per ASTM D1654 after removal from the kiln and placed in the salt drip tank. Even after sustaining 1000° F. in the kiln, the coating appeared to provide substantial protection of the steel surface against corrosion.

[0047] The salt dripping tests highlighted that the coating formed with the samples of the composition of the present invention was less soluble in fresh water than in salt water. To investigate the difference, the lower 2″ of two ceramic-coated steel coupons coated with the Example 1 composition were immersed in freshwater or saltwater for 100 days. The lower 2″ of each coupon was immersed. The coupon in fresh water was rust-stained (the back of the coupon was not coated), but the coating was otherwise intact. The coated portions of the freshwater specimen were well protected from corrosion (edges and back were not coated). The saltwater coupon was largely protected from corrosion (entire coupon was coated), however, much of the coating that was immersed in saltwater dissolved. Even in the dissolved area, however, the coupon was still mostly protected from corrosion, including along a scribe line.

EXAMPLE 1

Composition Makeup (Proportions by Volume)

Part A:

[0048] Hydrogen Hydroxide: 23.27% [0049] MKP: 64.5% [0050] Phosphoric Acid: 8% [0051] Methyl Cellulose: 0.13% [0052] Nanotized SiO.sub.2: 2% [0053] Nano Siloxane Complex: 0.1% [0054] Nanotized TiO.sub.2: 2%

Part B:

[0055] Hydrogen Hydroxide: 34% [0056] K.sub.3PO.sub.4: 3.8% [0057] Methyl Cellulose: 0.1% [0058] CaSiO.sub.3: 21% [0059] MgOH: 41% [0060] pH stabilizer Nonylphenol: 0.1%

[0061] The components of Part A and Part B of Example 1 were mixed together in the manner described above. Parts A and B were then mixed together in the manner described above. The usability test results indicated that the pH was too low, the composition of Example 1 did not spray well and slight outgassing was produced with resultant uneven finish. The functionality test results for surface protection and temperature resistance are presented above.

Example 2

Composition Makeup (Proportions by Volume)

Part A:

[0062] Hydrogen Hydroxide: 22.54% [0063] MKP: 64.5% [0064] Phosphoric Acid: 8.5% [0065] Methyl Cellulose: 0.16% [0066] Nanotized SiO.sub.2: 2.2% [0067] Nano Siloxane Complex: 0.1% [0068] Nanotized TiO.sub.2: 2%

Part B:

[0069] Hydrogen Hydroxide: 31% [0070] K.sub.3PO.sub.4: 4.4% [0071] Methyl Cellulose: 0.12% [0072] Metakaolin: 22% [0073] MgOH: 41% [0074] pH stabilizer Nonylphenol: 0.15%

[0075] The components of Part A and Part B of Example 2 were mixed together in the manner described above. Parts A and B were then mixed together in the manner described above. The usability test results indicated that the pH was satisfactory, the composition of Example 2 sprayed well with even distribution and a resultant smooth finish. The functionality test results indicated that surface protection was better for the Example 2 composition as compared to the example 1 composition, at least with respect to the salt drip test. It is believed that the Example 2 composition would be at least as effective as the Example 1 composition with respect to the other functionality testing conducted.

[0076] It was determined from the indicated initial testing that the composition of the present invention is suitable for conventional application by spraying, bonds well to the substrate and withstands environmental conditions with great protection of the substrate.

[0077] While the invention has been described with specific reference to particular components of the composition, certain versions representing specific combinations and the use of steps for making the composition, it is noted that the invention includes all reasonable equivalents.