A flame-retardant modified polyurethane coating and its preparation method

By combining phosphate-based nona isocyanate with nanotitanium dioxide, an organic-inorganic collaborative flame retardant system is formed, which solves the problem of insufficient flame retardant and antibacterial properties of polyurethane coatings and improves the comprehensive performance of the coatings.

CN120059589BActive Publication Date: 2025-08-05BEIXIN YUWANG WATERPROOF TECH (ANHUI) CO LTD
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Patent Information

Application Number
CN202510536998.5
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2025-04-27
Publication Date
2025-08-05
Estimated Expiration
2045-04-27

AI Technical Summary

Technical Problem

The poor flame retardant performance of existing polyurethane coatings limits its development and application in the field of flame retardant functionalization, and at the same time lacks antibacterial properties.

Method used

The phosphate-based nona isocyanate and nanotitanium dioxide are used to form an organic-inorganic collaborative flame retardant system, which improves the flame retardant performance through the phosphorus and nitrogen elements in the phosphate-based nona isocyanate, and the antibacterial performance is improved by using the trimeric quaternary ammonium structure, while the nanotitanium dioxide enhances the mechanical properties.

Benefits of technology

The obtained flame-retardant modified polyurethane coating has excellent flame retardant properties, antibacterial properties and mechanical properties. The combination of phosphate-based nona isocyanate and nanotitanium dioxide significantly improves the comprehensive performance of the coating.

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Abstract

The present invention relates to the technical field of coatings, and discloses a flame-retardant modified polyurethane coating and a preparation method thereof. The flame-retardant modified polyurethane coating of the present invention comprises component A and component B. Component A comprises raw materials in the following weight parts: 30-45 parts of polyether diol 2000D, 20-25 parts of polyether triol 330N, 15-30 parts of phosphate group nona-isocyanate; Component B comprises raw materials in the following weight parts: 2.5-19.5 parts of chlorinated paraffin, 0.2-0.5 part of dispersant 755W, 1-3 parts of 800-mesh heavy calcium, 1-4 parts of phosphate group nano-titanium dioxide, 0.5-1 part of leveling agent 100, 0.2-0.5 part of defoaming agent 810, 5 parts of propylene glycol methyl ether acetate, 0.1-0.3 part of dibutyltin dilaurate. Mix the two evenly to obtain the flame-retardant modified polyurethane coating. The flame-retardant modified polyurethane coating prepared by the present invention has excellent flame-retardant performance, antibacterial performance and mechanical properties.
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Description

Technical Field

[0001] The present invention relates to the technical field of coatings, and specifically relates to a flame-retardant modified polyurethane coating and a preparation method thereof. Background Art

[0002] Polyurethane coatings have good properties such as weather resistance and chemical resistance, and are widely used in fields such as woodware, automobiles, and waterproof coiled materials. However, the polyurethane has poor flame retardancy, and the lack of flame retardancy of polyurethane coatings limits their development and application in the field of flame-retardant functionalization. Therefore, under the condition of not affecting the original properties of polyurethane coatings, flame-retardant modification of polyurethane coatings is an urgent problem to be solved at present.

[0003] For example, the patent with the application publication number CN 118480305 A discloses a solvent-free exposed polyurethane waterproof and heat-insulating coating and a preparation method thereof. The invention uses cashew shell oil-modified polyol, polyacrylate polyol, oligophosphate flame retardant, modified nano-titanium dioxide, etc. as raw materials, and the prepared polyurethane coating has excellent flame retardancy and mechanical properties, but does not improve the antibacterial properties of the coating. Summary of the Invention

[0004] (I) Technical Problems to be Solved

[0005] Aiming at the deficiencies of the prior art, the present invention provides a flame-retardant modified polyurethane coating and a preparation method thereof. The prepared polyurethane coating not only has excellent flame retardancy, but also has excellent antibacterial properties and mechanical properties.

[0006] (II) Technical Solutions

[0007] A flame-retardant modified polyurethane coating, wherein the polyurethane coating comprises component A and component B;

[0008] Component A comprises the following raw materials in parts by weight: 30-35 parts of polyether diol 2000D, 20-25 parts of polyether triol 330N, 15-30 parts of phosphoric acid ester-based nona-isocyanate;

[0009] Component B comprises the following raw materials in parts by weight: 2.5-19.5 parts of chlorinated paraffin, 0.2-0.5 parts of dispersant 755W, 1-3 parts of 800-mesh heavy calcium, 1-4 parts of phosphoric acid ester-based nano-titanium dioxide, 0.5-1 part of leveling agent 100, 0.2-0.5 parts of defoaming agent 810, 5 parts of propylene glycol methyl ether acetate, 0.1-0.3 parts of dibutyltin dilaurate;

[0010] The preparation method of the phosphate group-functionalized nano-titanium dioxide is as follows: Disperse nano-titanium dioxide in an acetone solvent, add phosphate group-functionalized nona-isocyanate thereto, heat up to 70 - 80 °C, add dibutyltin dilaurate thereto, react for 1 - 2 h. After the reaction, wash with ethanol, centrifuge, and dry to obtain the phosphate group-functionalized nano-titanium dioxide.

[0011] Preferably, the dosage of the phosphate group-functionalized nona-isocyanate is 10 - 20% of the mass of the nano-titanium dioxide.

[0012] Preferably, the preparation method of the phosphate group-functionalized nona-isocyanate includes the following steps:

[0013] (1) Add 5-chloro-1-pentanol to a toluene solvent. Under nitrogen protection, add phosphorus pentoxide thereto, stir to disperse evenly, heat up to 90 - 100 °C, react for 10 - 14 h. After the reaction, perform vacuum distillation, wash with deionized water, and dry to obtain intermediate product 1;

[0014] (2) Add toluene diisocyanate and dibutyltin dilaurate to an acetone solvent, stir and mix evenly. At 30 - 40 °C, add triethanolamine and hydroquinone thereto, control the temperature at 45 - 50 °C, react for 3 - 5 h. After the reaction, evacuate to remove acetone, wash with deionized water, and dry to obtain intermediate product 2;

[0015] (3) Add intermediate product 1 and intermediate product 2 to a n-butanol solvent, stir to disperse, heat up to 60 - 70 °C, react for 18 - 24 h. After the reaction, perform rotary evaporation, wash with deionized water, and dry to obtain the phosphate group-functionalized nona-isocyanate.

[0016] Further preferably, in the step (1), the dosage ratio of 5-chloro-1-pentanol to phosphorus pentoxide is (2.5 - 3) g:1 g.

[0017] Further preferably, in the step (2), the dosage ratio of toluene diisocyanate to triethanolamine is (2.6 - 3.2) g:1 g.

[0018] Further preferably, in the step (2), the dosage of dibutyltin dilaurate is 0.5% of the mass of toluene diisocyanate; the dosage of hydroquinone is 0.2% of the mass of triethanolamine.

[0019] Further preferably, in the step (3), the dosage ratio of intermediate product 1 to intermediate product 2 is 1 g:(4.8 - 5.2) g.

[0020] The preparation method of the flame-retardant modified polyurethane coating includes the following steps:

[0021] (1) Vacuum dehydrate polyether diol 2000D and polyether triol 330N at 110 °C, cool down to 60 °C, add phosphoric acid ester group nona - isocyanate thereto, heat up to 90 °C, and react for 4 h to obtain Component A;

[0022] (2) Add dispersant 755W, 800 - mesh heavy calcium carbonate, phosphoric acid ester group nano - titanium dioxide into chlorinated paraffin, vacuum dehydrate at 110 °C for 2 h, cool down to room temperature, add leveling agent 100, defoamer 810, propylene glycol methyl ether acetate, dibutyltin dilaurate thereto, stir and degas for 1 h to obtain Component B;

[0023] (3) Mix Component A and Component B evenly to obtain the flame - retardant modified polyurethane coating.

[0024] (III) Beneficial technical effects

[0025] Reaction mechanism of the present invention: The present invention uses 5 - chloro - 1 - pentanol and phosphorus pentoxide as raw materials to obtain intermediate 1 through esterification. Using toluene diisocyanate, triethanolamine as raw materials, dibutyltin dilaurate as a catalyst, and hydroquinone as an inhibitor, through reaction, intermediate 2 is obtained. Utilize the chlorine contained in intermediate 1 to conduct quaternization reaction with the tertiary amine contained in intermediate 2 to obtain phosphoric acid ester group nona - isocyanate, which has nine isocyanate groups. Its structure is novel and the preparation method is simple. Utilize the isocyanate groups contained in phosphoric acid ester group nona - isocyanate to react with the hydroxyl groups on the surface of nano - titanium dioxide to obtain phosphoric acid ester group nano - titanium dioxide. React with polyether diol 2000D, polyether triol 330N, and phosphoric acid ester group nona - isocyanate as raw materials to obtain Component A, and stir and mix evenly with chlorinated paraffin, dispersant 755W, phosphoric acid ester group nano - titanium dioxide, dibutyltin dilaurate, etc. to obtain Component B. Finally, mix Component A and Component B evenly to obtain the flame - retardant modified polyurethane coating.

[0026] The phosphoric acid ester group nona - isocyanate prepared by the present invention contains organic flame - retardant elements, namely phosphorus element and nitrogen element. The phosphorus element can generate strongly dehydrating substances such as phosphoric acid when heated, and a dense isolation layer covers the surface of the coating, isolating the transportation of substances and energy; the nitrogen element generates non - flammable gases when heated, diluting the concentration of flammable gases in the air, and assisting in enhancing the flame - retardant performance. In addition, the heavy calcium carbonate and nano - titanium dioxide contained therein can be used as inorganic flame - retardant materials, forming an organic - inorganic synergistic flame - retardant system with organic flame - retardant materials to jointly enhance the flame - retardant effect of the material.

[0027] The prepared phosphoric acid ester-based nona-isocyanate of the present invention contains a trimeric quaternary ammonium salt structure, and its antibacterial effect is relatively better than that of the single quaternary ammonium salt structure and the gemini quaternary ammonium salt structure. Moreover, the present invention uses nano-titanium dioxide and trimeric quaternary ammonium salt to synergistically improve the antibacterial performance of polyurethane coatings, and the compounding of the two has a synergistic antibacterial effect on Escherichia coli and Staphylococcus aureus.

[0028] The nano-titanium dioxide used in the present invention has a small particle size and a large surface energy. Directly introducing it into the polyurethane coating is likely to cause agglomeration. The present invention uses phosphoric acid ester-based nona-isocyanate to treat nano-titanium dioxide, forming an organic-inorganic composite material with nano-titanium dioxide as the cross-linking point. This can not only reduce the agglomeration of nano-titanium dioxide, increase the compatibility, and make it evenly dispersed in the coating, but also, when subjected to impact, can absorb more impact energy as a stress concentration point, thus improving the mechanical properties of the material. In addition, the prepared phosphoric acid ester-based nona-isocyanate of the present invention contains more branched chain structures. When it is introduced into the polyurethane coating, its terminal isocyanate reacts with the hydroxyl group in the polyether alcohol, generating more urethane groups in the molecular chain, which can form a spatial cross-linked network structure. More molecular chains are cross-linked and entangled with each other, and the force between the molecular chains is enhanced, forming more chemical links and physical links, and then forming more cross-linking sites. When subjected to external impact, the impact force can be dispersed to other molecular chains along the cross-linking sites, thereby improving the mechanical properties of the polyurethane coating. The prepared polyurethane coating of the present invention has excellent flame retardant performance, antibacterial performance and mechanical properties. Brief Description of the Drawings

[0029] Figure 1 is the reaction route of intermediate 1;

[0030] Figure 2 is the reaction route of intermediate 2;

[0031] Figure 3 is the reaction route of phosphoric acid ester-based nona-isocyanate. Detailed Embodiments

[0032] Next, the technical solutions in the embodiments of the present invention will be clearly and completely described in conjunction with the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without making creative efforts belong to the scope of protection of the present invention. Example 1

[0033] (1) Add 12.5 g of 5-chloro-1-pentanol to toluene solvent. Under nitrogen protection, add 5 g of phosphorus pentoxide thereto, stir and disperse evenly, heat up to 95 °C, react for 12 h. After the reaction is completed, perform vacuum distillation, wash with deionized water, and dry to obtain intermediate 1.

[0034] (2) Add 30 g of toluene diisocyanate and 0.15 g of dibutyltin dilaurate to acetone solvent, stir and mix evenly. At 35 °C, add 10 g of triethanolamine and 0.02 g of hydroquinone thereto, control the temperature at 50 °C, react for 4 h. After the reaction is completed, evacuate to remove acetone, wash with deionized water, and dry to obtain intermediate 2.

[0035] (3) Add 5 g of intermediate 1 and 24 g of intermediate 2 to n-butanol solvent, stir and disperse, heat up to 70 °C, react for 18 h. After the reaction is completed, perform rotary evaporation, wash with deionized water, and dry to obtain phosphoric acid ester group nona-isocyanate.

[0036] (4) Disperse 5 g of nano-titanium dioxide in acetone solvent, add 0.5 g of phosphoric acid ester group nona-isocyanate thereto, heat up to 75 °C, add 10 drops of dibutyltin dilaurate thereto, react for 1 h. After the reaction is completed, wash with ethanol, centrifuge, and dry to obtain phosphoric acid ester group nano-titanium dioxide.

[0037] (5) By weight, vacuum dehydrate 35 parts of polyether diol 2000D and 20 parts of polyether triol 330N at 110 °C, cool down to 60 °C, add 15 parts of phosphoric acid ester group nona-isocyanate thereto, heat up to 90 °C, react for 4 h to obtain component A.

[0038] (6) By weight, add 0.2 part of dispersant 755W, 3 parts of 800-mesh heavy calcium, 1 part of phosphoric acid ester group nano-titanium dioxide to 19.5 parts of chlorinated paraffin, vacuum dehydrate at 110 °C for 2 h, cool down to room temperature, add 0.5 part of leveling agent 100, 0.5 part of defoaming agent 810, 5 parts of propylene glycol methyl ether acetate, 0.3 part of dibutyltin dilaurate thereto, stir and degas for 1 h to obtain component B.

[0039] (7) Mix component A and component B evenly to obtain a flame-retardant modified polyurethane coating. Example 2

[0040] (1) Add 14 g of 5-chloro-1-pentanol to toluene solvent. Under nitrogen protection, add 5 g of phosphorus pentoxide thereto, stir and disperse evenly, heat up to 100 °C, react for 10 h. After the reaction is completed, perform vacuum distillation, wash with deionized water, and dry to obtain intermediate 1.

[0041] (2) Add 32 g of toluene diisocyanate and 0.16 g of dibutyltin dilaurate to acetone solvent, stir and mix evenly. At 30 °C, add 10 g of triethanolamine and 0.02 g of hydroquinone thereto, control the temperature at 50 °C, react for 3 h. After the reaction is completed, remove acetone by vacuum, wash with deionized water, and dry to obtain intermediate product 2.

[0042] (3) Add 5 g of intermediate product 1 and 25 g of intermediate product 2 to n-butanol solvent, stir and disperse, heat up to 60 °C, react for 24 h. After the reaction is completed, perform rotary evaporation, wash with deionized water, and dry to obtain phosphoric acid ester group nona-isocyanate.

[0043] (4) Disperse 5 g of nano-titanium dioxide in acetone solvent, add 0.8 g of phosphoric acid ester group nona-isocyanate thereto, heat up to 75 °C, add 10 drops of dibutyltin dilaurate thereto, react for 1.5 h. After the reaction is completed, wash with ethanol, centrifuge, and dry to obtain phosphoric acid ester group nano-titanium dioxide.

[0044] (5) By weight, vacuum dehydrate 30 parts of polyether diol 2000D and 25 parts of polyether triol 330N at 110 °C, cool down to 60 °C, add 20 parts of phosphoric acid ester group nona-isocyanate thereto, heat up to 90 °C, react for 4 h to obtain component A.

[0045] (6) By weight, add 0.2 part of dispersant 755W, 3 parts of 800-mesh heavy calcium, 2 parts of phosphoric acid ester group nano-titanium dioxide to 13.3 parts of chlorinated paraffin, vacuum dehydrate at 110 °C for 2 h, cool down to room temperature, add 1 part of leveling agent 100, 0.2 part of defoaming agent 810, 5 parts of propylene glycol methyl ether acetate, 0.3 part of dibutyltin dilaurate thereto, stir and degas for 1 h to obtain component B.

[0046] (7) Mix component A and component B evenly to obtain flame retardant modified polyurethane coating. Example 3

[0047] (1) Add 15 g of 5-chloro-1-pentanol to toluene solvent, under nitrogen protection, add 5 g of phosphorus pentoxide thereto, stir and disperse evenly, heat up to 90 °C, react for 14 h. After the reaction is completed, perform vacuum distillation, wash with deionized water, and dry to obtain intermediate product 1.

[0048] (2) Add 30 g of toluene diisocyanate and 0.15 g of dibutyltin dilaurate to acetone solvent, stir and mix evenly. At 40 °C, add 10 g of triethanolamine and 0.02 g of hydroquinone thereto, control the temperature at 45 °C, react for 4 h. After the reaction is completed, remove acetone by vacuum, wash with deionized water, and dry to obtain intermediate product 2.

[0049] (3) Add 5 g of intermediate 1 and 26 g of intermediate 2 to n-butanol solvent, stir and disperse, heat up to 65 °C, react for 20 h. After the reaction, perform rotary evaporation, wash with deionized water, and dry to obtain phosphoric acid ester group nona-isocyanate.

[0050] (4) Disperse 5 g of nano-titanium dioxide in acetone solvent, add 0.9 g of phosphoric acid ester group nona-isocyanate thereto, heat up to 80 °C, add 10 drops of dibutyltin dilaurate thereto, react for 1 h. After the reaction, wash with ethanol, centrifuge, and dry to obtain phosphoric acid ester group nano-titanium dioxide.

[0051] (5) By weight, vacuum dehydrate 35 parts of polyether diol 2000D and 20 parts of polyether triol 330N at 110 °C, cool down to 60 °C, add 25 parts of phosphoric acid ester group nona-isocyanate thereto, heat up to 90 °C, and react for 4 h to obtain Component A.

[0052] (6) By weight, add 0.5 part of dispersant 755W, 1 part of 800-mesh heavy calcium carbonate, 3 parts of phosphoric acid ester group nano-titanium dioxide to 9.7 parts of chlorinated paraffin, vacuum dehydrate at 110 °C for 2 h, cool down to room temperature, add 0.5 part of leveling agent 100, 0.2 part of defoaming agent 810, 5 parts of propylene glycol methyl ether acetate, 0.1 part of dibutyltin dilaurate thereto, stir and degas for 1 h to obtain Component B.

[0053] (7) Mix Component A and Component B evenly to obtain flame-retardant modified polyurethane coating. Example 4

[0054] (1) Add 14 g of 5-chloro-1-pentanol to toluene solvent, under nitrogen protection, add 5 g of phosphorus pentoxide thereto, stir and disperse evenly, heat up to 95 °C, react for 12 h. After the reaction, perform vacuum distillation, wash with deionized water, and dry to obtain intermediate 1.

[0055] (2) Add 26 g of toluene diisocyanate and 0.13 g of dibutyltin dilaurate to acetone solvent, stir and mix evenly, at 35 °C, add 10 g of triethanolamine and 0.02 g of hydroquinone thereto, control the temperature at 50 °C, react for 5 h. After the reaction, evacuate to remove acetone, wash with deionized water, and dry to obtain intermediate 2.

[0056] (3) Add 5 g of intermediate 1 and 25 g of intermediate 2 to n-butanol solvent, stir and disperse, heat up to 70 °C, react for 18 h. After the reaction, perform rotary evaporation, wash with deionized water, and dry to obtain phosphoric acid ester group nona-isocyanate.

[0057] (4) Disperse 5 g of nano-titanium dioxide in acetone solvent, add 1 g of phosphoric acid ester group nona-isocyanate thereto, heat up to 70 °C, add 10 drops of dibutyltin dilaurate thereto, react for 2 h, after the reaction is completed, wash with ethanol, centrifuge, and dry to obtain phosphoric acid ester group nano-titanium dioxide.

[0058] (5) By weight, vacuum dehydrate 35 parts of polyether diol 2000D and 20 parts of polyether triol 330N at 110 °C, cool down to 60 °C, add 30 parts of phosphoric acid ester group nona-isocyanate thereto, heat up to 90 °C, and react for 4 h to obtain Component A.

[0059] (6) By weight, add 0.4 part of dispersant 755W, 2 parts of 800-mesh heavy calcium carbonate, 4 parts of phosphoric acid ester group nano-titanium dioxide to 2.5 parts of chlorinated paraffin, vacuum dehydrate at 110 °C for 2 h, cool down to room temperature, add 0.5 part of leveling agent 100, 0.3 part of defoaming agent 810, 5 parts of propylene glycol methyl ether acetate, and 0.3 part of dibutyltin dilaurate thereto, stir and degas for 1 h to obtain Component B.

[0060] (7) Mix Component A and Component B evenly to obtain a flame-retardant modified polyurethane coating.

[0061] Comparative Example 1

[0062] The flame-retardant modified polyurethane coating and its preparation method provided in this comparative example are generally the same as those in Example 1, and the main difference is that: Comparative Example 1 does not contain phosphoric acid ester group nano-titanium dioxide.

[0063] Comparative Example 2

[0064] The flame-retardant modified polyurethane coating and its preparation method provided in this comparative example are generally the same as those in Example 1, and the main difference is that: Comparative Example 1 replaces the phosphoric acid ester group nona-isocyanate in Example 1 with toluene diisocyanate.

[0065] Apply the coating on tinplate and dry it in an oven at 80 °C to form a coating film.

[0066] Use a limiting oxygen index tester to test the oxygen index of the coating, and the specimen size is 120 mm × 6 mm × 3 mm.

[0067] Use a universal tensile machine to test the tensile properties of the coating, and the tensile speed is 100 mm / min.

[0068] Use a film impact tester to test the impact resistance.

[0069] Table 1: Test results of the flame-retardant properties and mechanical properties of each example and comparative example

[0070]

[0071] As can be seen from the table, the polyurethane coating prepared by the present invention has excellent flame retardant properties and mechanical properties.

[0072] Referring to GB / T21866-2008, the antibacterial properties of the coating were tested.

[0073] Table 2: Antibacterial test results of each example and comparative example

[0074]

[0075] As can be seen from the table, the polyurethane coating prepared by the present invention has good antibacterial properties, and with the increase of the dosage of phosphate group nano-titanium dioxide and phosphate group nona-isocyanate, the antibacterial property can reach up to 99.9%.

[0076] In the description of the specification, the description of reference terms such as "one embodiment", "example", "specific example", etc. means that the specific features, structures, materials or characteristics described in connection with the embodiment or example are included in at least one embodiment or example of the present invention. In this specification, the schematic representations of the above terms do not necessarily refer to the same embodiment or example. Moreover, the specific features, structures, materials or characteristics described can be combined in a suitable manner in any one or more embodiments or examples.

Claims

1. A flame retardant modified polyurethane coating, characterized in that: The polyurethane coating comprises component A and component B; The A component includes the following raw materials in parts by weight: 30-35 parts of polyether diol 2000D, 20-25 parts of polyether triol 330N, and 15-30 parts of phosphate nonaisocyanate; The B component includes the following raw materials in parts by weight: 2.5-19.5 parts of chlorinated paraffin, 0.2-0.5 parts of dispersant 755W, 1-3 parts of 800 mesh heavy calcium, 1-4 parts of phosphate-based nano titanium dioxide, 0.5-1 parts of leveling agent 100, 0.2-0.5 parts of defoamer 810, 5 parts of propylene glycol methyl ether acetate, and 0.1-0.3 parts of dibutyltin dilaurate; The preparation method of the phosphate-based nano-titanium dioxide comprises: dispersing nano-titanium dioxide in an acetone solvent, adding phosphate-based nonaisocyanate thereto, heating to 70-80° C., adding dibutyltin dilaurate thereto, reacting for 1-2 hours, washing with ethanol after the reaction, centrifuging, and drying to obtain the phosphate-based nano-titanium dioxide; The preparation method of the phosphate nonaisocyanate comprises the following steps: (1) Add 5-chloro-1-pentanol to toluene solvent, add phosphorus pentoxide under nitrogen protection, stir and disperse evenly, heat to 90-100°C, react for 10-14 hours, and after the reaction is completed, distill under reduced pressure, wash with deionized water, and dry to obtain intermediate 1; (2) Toluene diisocyanate and dibutyltin dilaurate were added to acetone solvent, stirred and mixed evenly, and triethanolamine and hydroquinone were added thereto at 30-40°C, and the temperature was controlled at 45-50°C. The reaction was carried out for 3-5 hours. After the reaction was completed, the acetone was removed by vacuum, and the mixture was washed with deionized water and dried to obtain intermediate product 2; (3) Add intermediate product 1 and intermediate product 2 to n-butanol solvent, stir and disperse, heat to 60-70°C, react for 18-24 hours, and after the reaction is completed, rotary evaporate, wash with deionized water, and dry to obtain phosphate nonaisocyanate.

2. The flame retardant modified polyurethane coating according to claim 1, characterized in that: In the preparation of phosphate-based nano-titanium dioxide, the amount of the phosphate-based nonaisocyanate is 10-20% of the mass of the nano-titanium dioxide.

3. The flame retardant modified polyurethane coating according to claim 1, characterized in that: In the above (1), the usage ratio of 5-chloro-1-pentanol and phosphorus pentoxide is (2.5-3) g:1 g.

4. The flame retardant modified polyurethane coating according to claim 1, characterized in that: In the above (2), the usage ratio of toluene diisocyanate and triethanolamine is (2.6-3.2) g:1 g.

5. The flame retardant modified polyurethane coating according to claim 1, characterized in that: In (2), the amount of dibutyltin dilaurate used is 0.5% of the mass of toluene diisocyanate; the amount of hydroquinone used is 0.2% of the mass of triethanolamine.

6. The flame retardant modified polyurethane coating according to claim 1, characterized in that: In the above (3), the usage ratio of intermediate product 1 and intermediate product 2 is 1g:(4.8-5.2)g.

7. The method for preparing a flame retardant modified polyurethane coating according to any one of claims 1 to 6, characterized in that: The following steps are involved: (1) Polyether diol 2000D and polyether triol 330N were vacuum dehydrated at 110°C, cooled to 60°C, and phosphate nonaisocyanate was added thereto. The temperature was raised to 90°C and the reaction was carried out for 4 hours to obtain component A. (2) Dispersant 755W, 800 mesh heavy calcium, and phosphate-based nano-titanium dioxide were added to chlorinated paraffin, vacuum dehydrated at 110°C for 2 hours, cooled to room temperature, and leveling agent 100, defoamer 810, propylene glycol methyl ether acetate, and dibutyltin dilaurate were added thereto, and stirred and degassed for 1 hour to obtain component B; (3) Component A and component B are mixed evenly to obtain a flame retardant modified polyurethane coating.

Citation Information

Patent Citations

  • Solvent-free exposed polyurethane waterproof heat-insulating coating and preparation method thereof

    CN118480305A