3 lines
20 KiB
JSON
3 lines
20 KiB
JSON
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"protocol": "The anti-fog polyurethane coating compositions are applied directly to a substrate or directly to a primer-coated substrate and cured, or the coating compositions are cast into unsupported films for later attachment to the substrate.Surfactants can be mixed into the polyurethane coating composition before application to a substrate. This allows the surfactant to become physically trapped within the polyurethane polymer structure during the curing process.1. Prepare a first polyurethane using a diol with polyethylene oxide side chain segments, an additional polyol component, a first polyisocyanate, and a dihydroxy-carboxylic acid neutralized with a carboxylic-reactive amphoteric surfactant to form a salt. 2. Mix the first polyurethane with a liquid phase (water, organic solvent, or a combination). 3. Prepare a second polyurethane from a second polyol and an additional polyol component, a partially blocked tri-functional polyisocyanate, an isocyanate-reactive salt of a surfactant, and an isocyanate-reactive cationic surfactant. 4. Incorporate hydrophilic main chain or side chain segments in the polyurethanes at a concentration of 0.01% to 40% by weight of the solids. 5. Adjust the composition as needed for the desired properties.The synthesis of the third polyurethane involves the reaction of a third polyol component, which includes a diol with polyethylene oxide side chain segments and an additional different polyol, with a third polyisocyanate component. The third polyisocyanate comprises at least one polyisocyanate from the group of diisocyanates, triisocyanates, or their derivatives, and at least one partially blocked tri-functional polyisocyanate. The resulting polyurethane should contain hydrophilic main chain segments or hydrophilic side chain segments in an amount ranging from about 0.01% to about 40% by weight of the solids of the polyurethane.The synthesis of hydrophilic polymers with functional groups involves the following steps: 1. Combine a diol containing polyethylene oxide side chain segments with at least one other different polyol in a reaction mix. 2. Introduce a polyisocyanate into the reaction mix, ensuring the ratio of isocyanate functional groups to hydroxyl functional groups is greater than or equal to about 1.1:1. 3. Incorporate a dihydroxy-carboxylic acid into the reaction mix. 4. Allow the reaction to occur in a suitable organic solvent at high temperatures, leading to the formation of a polyurethane with carboxylic acid functional groups. 5. Introduce a carboxylic-reactive amphoteric surfactant to the reaction mixture to neutralize the carboxylic acid functional groups, resulting in a salt of the amphoteric surfactant chemically bonded to the polyurethane. 6. The final polyurethane structure will have hydrophilic segments that contribute to its dispersibility and anti-fog properties.To synthesize hydrophilic polymers with functional groups, the following steps should be taken: 1) Combine a liquid phase consisting of either water, an organic solvent, or combinations thereof with a polyurethane. 2) The polyurethane is formed from the reaction of polyols such as: (a) diols with main chain segments from polyethylene oxide and/or polypropylene oxide, (b) triols with similar segments, and (c) at least one additional different polyol. Ensure the polyol used has hydrophilic main chain segments, preferably comprising polyethylene oxide or polypropylene oxide, in amounts between 0.01% and 40% by weight of the solids of polyurethane. 3) Incorporate at least one partially blocked tri-functional polyisocyanate into the system. The polyisocyanates should comprise between 5% and 60% of the weight of the solids of the polyurethane. 4) Introduce an isocyanate-reactive salt of a surfactant, preferably mono-functional, accounting for 0.1% to 7% by weight of solids. 5) Add an isocyanate-reactive cationic surfactant, which should constitute 0.1% to 20% by weight of the solids and should contain at least one isocyanate-reactive functional group. 6) Catalysts, such as metal carboxylates, can be introduced to aid the reaction. 7) Once the mixture is prepared, agitate mechanically to disperse the prepolymer into the liquid phase, aiding the formation of a stable colloidal dispersion. 8) Perform a final polymerization step where the isocyanate-terminated prepolymer reacts with chain extenders to yield a higher molecular weight polyurethane. These extenders may include multifunctional amines or polyols. 9) The final product can then be applied to various substrates using methods such as flow coating or spray coating.The synthesis of hydrophilic polymers with functional groups is performed by applying an aqueous polyurethane dispersion to polycarbonate lenses. Specifically, five or six polycarbonate lenses are dip-coated in the aqueous polyurethane dispersion at a draw speed of 12 inches per minute. After dip-coating, the lenses are allowed to dry and may undergo pre-curing conditions before the final curing step. The curing is conducted by treating the coated lenses with heat at a designated temperature for a specified duration. The selection of polyurethane coated lenses varies based on the tests to be performed, ensuring that different coated lenses are utilized for adhesion and anti-fogging assessments.To synthesize the PEO side-chained diol, a two-step reaction is conducted. In the first step, hexamethylene diioscyanate is reacted with a mono-methyoxy-polyethylene glycol with an average molecular weight (Mn) of about 1,000. After the mono-functional mono-methyoxy-polyethylene glycol reacts with one isocyanate functional group of the diisocyanate, the remaining isocyanate functional group is then reacted with diethanolamine to yield the final diol product. This diol compound possesses polyethylene oxide side chains.21.1 grams (g) of IPDI, 28.2 g of PC 2000, 2.1 g of trimethylolpropane, 3.2 g of dimethylolpropionic acid, 8.1 g of Tegomer D3403, and 35 g of methylethylketone are mixed together. The mixture is heated to 70°C, and 0.01 g of tin 6: catalyst is added. The mixture is then reacted for 3 hours in a nitrogen environment. After the reaction finishes, the resulting polyurethane prepolymer mixture is cooled to 40°C. 40.3 g of polyurethane prepolymer mixture is then dispersed into 51.2 g of water and 7.0 g of aqueous betaine surfactant solution with a high shear disperser. 0.25 g of hydrazine-monohydrate and 0.58 g of 1,6-hexanediamine are also added during dispersion with the high shear disperser, resulting in an aqueous polyurethane dispersion having about 27% solids by weight of the dispersion. The resulting polyurethane comprises about 10% polyethylene oxide side chains by weight of the solids of the polyurethane and about 10% neutralized amines by weight of the solids of the polyurethane.Mix $24.7\\mathrm{g}$ of IPDI, $14.7\\mathrm{g}$ of PC 2000, $3.2\\mathrm{g}$ of trimethylolpropane, $3.0\\mathrm{g}$ of dimethylolpropionic acid, $15.3\\mathrm{g}$ of PEO-side chained diol, $1.9\\mathrm{g}$ of PTF 1000, and $35\\mathrm{g}$ of acetonitrile. Heat the mixture to $70^{\\circ}\\mathrm{C}$ and add $0.01\\mathrm{g}$ of tin catalyst. React for 3 hours in a nitrogen environment. After the reaction, cool the resulting polyurethane prepolymer mixture to $40^{\\circ}\\mathrm{C}$. Disperse $40.9\\mathrm{g}$ of the polyurethane prepolymer mixture into $51.2\\mathrm{g}$ of water and $7.4\\mathrm{g}$ of aqueous amine oxide surfactant solution using a high shear disperser. Add $0.55\\mathrm{g}$ of hydrazinemonohydrate during dispersion. Resulting in an aqueous polyurethane dispersion having about $28\\%$ solids by weight. The resulting polyurethane comprises about $17\\%$ polyethylene oxide side chains by weight and about $8\\%$ neutralized amines by weight of the solids. Measure viscosity at $25^{\\circ}\\mathrm{C}$, which is 39 cps. Dip-coat a polycarbonate lens in the aqueous polyurethane dispersion at a 12 inch/min draw speed. Dry for $30\\mathrm{min}$ at room temperature, resulting in a tack-free coating. Cure the coated lens at $90^{\\circ}\\mathrm{C}$ for 2 hours. The resulting coating thickness is about $11.5\\upmu\\mathrm{m}$.Dissolve 22.0 g of IPDI, 20.2 g of PC 2000, 2.1 g of trimethylolpropane, 3.2 g of dimethylolpropionic acid, and 9.1 g of PEO-side in an appropriate solvent. Stir the mixture until completely homogeneous to prepare the aqueous polyurethane dispersion containing functional groups.Mix 5.9 g of PEG 1000 and 35 g of methylethylketone, then heat the mixture to 70°C. Add 0.01 g of tin catalyst and react for 3 hours in a nitrogen environment. Allow the reaction to cool to 40°C. Disperse 37.2 g of the polyurethane prepolymer mixture into 53.3 g of water and 7.3 g of aqueous amine oxide surfactant solution using a high shear disperser. During dispersion, add 0.25 g of hydrazine-monohydrate and 0.59 g of 1,6-hexanediamine. This will result in an aqueous polyurethane dispersion with about 27% solids by weight. The dispersion contains approximately 10% polyethylene oxide side chains, 10% polyethylene oxide main chains, and 8% neutralized amines by weight of the solids. The measured viscosity of the dispersion should be 63 cps at 25°C. Dip-coat a polycarbonate lens in the dispersion at a 12 inch/min draw speed. Dry the dip-coated lens for 30 minutes at room temperature, resulting in a tack-free coating. Cure the coated lens at 90°C for 2 hours, achieving a coating thickness of about 11.0 μm.To synthesize hydrophilic polymers with functional groups, mix 21.8 g of IPDI, 19.0 g of PC 2000, 2.1 g of trimethylolpropane, 3.2 g of dimethylolpropionic acid, 9.1 g of PEO-side chained diol, 5.9 g of PEG 1000, and 35 g of methylethylketone. Heat the mixture to 70°C and add 0.01 g of tin catalyst. React for 3 hours in a nitrogen environment. Cool the mixture to 40°C and add 1.4 g of Trixene BI 7961. Disperse 37.1 g of the resulting polyurethane prepolymer mixture into 53.4 g of water and 7.3 g of aqueous amine oxide surfactant solution using a high shear disperser. Add 0.25 g of hydrazine-monohydrate and 0.59 g of 1,6-hexanediamine during dispersion. The final dispersion should contain about 25% solids by weight. For the polycarbonate lens application, dip-coat at a 12 inch/min draw speed, dry at room temperature for 30 minutes, and cure at 90°C for 2 hours. Alternatively, for the polyurethane mixture with an isocyanate-reactive salt, mix 24.7 g of Trixene DP9C/012, 4.2 g of Poly G 83-34, 1.1 g of Pluronic L-62, 0.5 g of trimethylolethane, 0.6 g of triethanolamine, and 5.0 g of DMAMP DBS solution with 4.1 g of N-methyl pyrrolidone, 4.5 g of tertiary amyl alcohol, 7.9 g of methylethylketone, and 0.9 g of 2-pentanedione. Heat to 60°C and react for 8 hours in a nitrogen environment, then cool to 30°C.35 g Trixene DP9C/012, 1.2 g PEG 1000, 4.6 g PC 2000, 0.6 g trimethylolpropane, 3.8 g Tegomer D3403, 1.2 g Cirrasol G-265, and 0.002 g tin catalyst are added to 4.0 g methylethylketone and 2.8 g diacetone alcohol and are mixed together. The mixture is heated to 60°C and then reacted for 6 hours in a nitrogen environment. Following the reaction, the resulting polyurethane prepolymer mixture is cooled to 30°C. The polyurethane prepolymer mixture is then dispersed in 63.0 g of distilled water, 0.34 g 1,6-hexanediamine, and 0.15 g 30% aqueous hydrazine with a high shear disperser, resulting in a stable aqueous polyurethane dispersion having about 24% solids by weight of the dispersion.Add 4.6 g IPDI, 5.5 g DP9C/012, 7.8 g PC 2000, 0.7 g trimethylolpropane, 3.2 g PEO-side chained diol, 2.1 g Cirrasol G-265, and 0.011 g tin catalyst to 10.3 g N-methyl pyrrolidone and 2.2 g diacetone alcohol. Mix and heat to 65°C, then react for 3 hours in an inert atmosphere. Cool the mixture to 40°C, then disperse in 66.6 g distilled water and 0.65 g (2-aminoethyl) aminoethanol using a high shear disperser, obtaining a stable aqueous polyurethane dispersion with about 24% solids. Resulting polyurethane comprises about 11% polyethylene oxide side chains, about 2% polyethylene oxide main chains, and about 11.7% blocked polyisocyanates by weight of solids. For dip-coating, use a draw speed of 12 inch/min and cure at 120°C for 1 hour, aiming for a thickness of about 8.1 µm.To prepare the hydrophilic polymer, mix 3.1 g of IPDI, 3.6 g of DP9C/012, 3.0 g of PC 2000, 0.3 g of trimethylolpropane, 2.3 g of PEO side-chained diol, 1.0 g of Poly G 83-34, 1.3 g of Cirrasol G-265, 0.7 g of DMAMP DBS solution, 0.9 g of sodium dioctylsulfosuccinate, and 0.011 g of tin catalyst in 5.1 g of N-methyl pyrrolidone and 2.2 g of diacetone alcohol. Heat this mixture to 65°C and react for 3 hours in an inert atmosphere. After the reaction, cool the resulting polyurethane prepolymer mixture to 40°C. Then, disperse the cooled mixture in 75.7 g of distilled water and 0.4 g of 2-(2-aminoethyl)aminoethanol using a high shear disperser, resulting in a stable aqueous polyurethane dispersion with about 16% solids by weight. The final polymer composition includes about 12% polyethylene oxide side chains, 6% polyethylene oxide main chains, and 11% blocked polyisocyanates by weight of the solids.100 g of the aqueous polyurethane dispersion from Example 8 is mixed with 100 g of the aqueous polyurethane dispersion from Example 3.To synthesize the hydrophilic polyurethane, prepare an aqueous polyurethane dispersion containing 25% solids by weight. To reduce viscosity, add 100 g of water with agitation until a stable, hazy dispersion with about 17% solids by weight is achieved. The resulting polyurethane should consist of 6.7% polyethylene oxide side chains, 10.9% polyethylene oxide main chains, 4.2% neutralized amines, and 22.6% blocked polyisocyanates by weight of the solids. Next, dip-coat a polycarbonate lens in the dispersion at a draw speed of 12 inches/min. Dry the dip-coated lens at room temperature for 5 minutes, then at 85°C for an additional 10 minutes until tack-free. Cure the tack-free coated lens at 120°C for 1 hour, resulting in a coating thickness of about 8.1 µm.50 g of the prepolymer of Example 3 and 50 g of the prepolymer of Example 8 are mixed together and added to 185.5 g 1-methoxy-2-propanol with agitation, resulting in a homogenous, clear polyurethane solution. The polyurethane solution comprises essentially all non-aqueous solvents and has about 20% solids by weight. The resulting polyurethane comprises about 9.0% polyethylene oxide side chains, about 11.5% polyethylene oxide main chains, and about 22.6% blocked polyisocyanates by weight of the solids. The viscosity of the solution is about 25 cps at 25°C. A polycarbonate lens is dip-coated in the polyurethane solution at a 12 inch/min draw speed, dried at room temperature for 5 minutes, then at 85°C for an additional 10 minutes. The coated lens is cured at 120°C for 1 hour, resulting in a coating with a thickness of about 5.8 μm.50 g of the prepolymer of Example 3 and 50 g of the prepolymer of Example 8 are mixed together and added to a mixture of 93 g 1-methoxy-2-propanol and 93 g water. 5.8 g aqueous amine oxide surfactant solution, 0.20 g hydrazine monohydrate, and 0.47 g hexanediamine chain extenders are added to the prepolymer mixture with agitation, resulting in a hazy aqueous polyurethane dispersion and an organic solvent polyurethane solution mixture. The resulting polyurethane mixture has a solid content of about 20% by weight of the polyurethane mixture. A polycarbonate lens is dip-coated in the aqueous polyurethane dispersion at a 12 inch/min draw speed. The dip-coated lens is dried at room temperature for 5 minutes and then dried at 85°C for an additional 10 minutes. The tack-free coated lens is cured at 120°C for 1 hour.Mix 23.3 g of IPDI, 7.1 g of PC 2000, 2.1 g of trimethylolpropane, 29.6 g of Tegomer D3403, 2.8 g of 1,6-hexanediol, and 35 g of acetonitrile together. Heat the mixture to 70°C, then add 0.01 g of tin catalyst. React the mixture for 3 hours in a nitrogen environment. After the reaction, cool the resulting polyurethane prepolymer mixture to 40°C. Disperse 45.2 g of the cooled polyurethane prepolymer mixture in 51.7 g of water using a high shear disperser. Add 0.62 g of hydrazine-monohydrate during dispersion. The resulting aqueous polyurethane dispersion will have about 30% solids by weight and comprise about 40% polyethylene oxide side chains by weight of the solids. Measure the viscosity of the dispersion, which is 70 cps at 25°C. Dip-coat a polycarbonate lens in the dispersion at a draw speed of 12 inches/min. Dry the dip-coated lens for 30 minutes at room temperature and cure at 90°C for 2 hours, resulting in a coating thickness of about 18.0 µm.$22.9\\mathrm{g}$ of IPDI, $14.5\\mathrm{g}$ of PC 2000, $2.2\\mathrm{g}$ of trimethylolpropane, $22.6\\mathrm{g}$ of Tegomer D3403, $2.9\\:\\mathrm{g}$ of 1,6-hexanediol, and $35\\mathrm{g}$ of acetonitrile are mixed together. The mixture is heated to $70^{\\circ}\\mathrm{C}.$ $_{0.01\\mathrm{~g~}}$ of tin catalyst is added. The mixture is then reacted for 3 hours in a nitrogen environment. After the reaction finishes, the resulting polyurethane prepolymer mixture is cooled to $40^{\\circ}$ C. $_{45.2\\mathrm{~g~}}$ of the cooled polyurethane prepolymer mixture is dispersed in $51.7\\mathrm{g}$ of water with a high shear disperser. $\\mathbf{0.62\\g}$ of hydrazine-monohydrate is also added during dispersion with the high shear disperser, resulting in an aqueous polyurethane dispersion having about $30\\%$ solids by weight of the dispersion.$21.6\\ \\mathrm{g}$ of IPDI, $31.0\\mathrm{g}$ of PC 2000, $2.1\\ \\mathrm{g}$ of trimethylolpropane, $7.4\\ \\mathrm{g}$ of Tegomer D3403, $2.8\\ \\mathrm{g}$ of 1,6-hexanediol, and $35\\mathrm{g}$ of acetonitrile are mixed together. The mixture is heated to $70^{\\circ}\\mathrm{C}$, and $0.01\\ \\mathrm{g}$ of tin catalyst is added. The mixture is then reacted for 3 hours in a nitrogen environment. After the reaction finishes, the resulting polyurethane mixture is cooled to $40^{\\circ}\\mathrm{C}$. $_{45.2\\mathrm{~g~}}$ of the cooled polyurethane mixture fails to disperse in $51.8\\ \\mathrm{g}$ of water with a high shear disperser. The resulting polyurethane comprises about $10\\%$ polyethylene oxide side chains by weight of the solids of the polyurethane.$25.4 g of IPDI, $24.8 g of PC 2000, $0.5 g of trimethylolpropane, $4.0 g of dimethylolpropionic acid, $9.9 g of Tegomer D3403, $2.5 g of 1,6-hexanediol, and $30 g of acetonitrile are mixed together. The mixture is heated to $70^{\\circ}C$, and $0.01 g$ of tin catalyst is added. The mixture is then reacted for 3 hours in a nitrogen environment. After the reaction finishes, the resulting polyurethane mixture is cooled to $40^{\\circ} C$. $27.9 g$ of the cooled polyurethane mixture fails to disperse into a mixture of $47.4 g$ of water and $24.8 g$ of quaternary amine surfactant solution with high shear disperser. The resulting polyurethane comprises about $12\\%$ polyethylene oxide side chains by weight of the solids of the polyurethane and about $10\\%$ neutralized amine by weight of the solids of the polyurethane.Mix 22.2 g of IPDI, 22.8 g of PC 2000, 2.1 g of trimethylolpropane, 15.0 g of Tegomer D3403, 2.8 g of 1,6-hexanediol, and 35 g of acetonitrile together. Heat the mixture to 70°C and add 0.01 g of tin catalyst. React for 3 hours in a nitrogen environment. After the reaction, cool the resulting polyurethane prepolymer mixture to 40°C. disperse 45.2 g of the cooled polyurethane prepolymer mixture in 51.8 g of water using a high shear disperser. Add 0.60 g of hydrazine-monohydrate during dispersion. The result will be an aqueous polyurethane dispersion with about 30% solids by weight. This polyurethane will comprise about 20% polyethylene oxide side chains by weight of the solids.The synthesis involves the composition of a first polyisocyanate component that may include a blocked polyisocyanate, and a second polyisocyanate component selected from diisocyanates and triisocyanates. Additionally, the synthesis uses a partially blocked tri-functional polyisocyanate with 1 free isocyanate functional group and 2 blocked isocyanate functional groups. An isocyanate-reactive salt of a surfactant is created through a neutralization reaction between an anionic surfactant's acid and a base containing an isocyanate-reactive functional group. Specific examples include a quaternary ammonium surfactant with 2 hydrophilic isocyanate-reactive functional groups and a hydrocarbon chain of at least 18 carbon atoms. The organic solvent utilized can comprise a variety of substances such as ketones, esters, or glycol ethers. Moreover, the process involves applying the coating composition to a substrate and curing it to create a durable coating."
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