A bio-based aspartame polyurea seam beautifying agent and its preparation method
By combining bio-based materials and modified hollow glass microspheres, an asparagus polyurea caulking agent with excellent performance was prepared, which solved the shortcomings of bio-based caulking agents in performance stability and environmental protection, and achieved efficient and safe construction effects.
Patent Information
- Application Number
- CN202411018653.2
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2024-07-29
- Publication Date
- 2025-09-09
- Estimated Expiration
- 2044-07-29
AI Technical Summary
Bio-based asparagus polyurea caulking agent has defects in production process, formula adjustment and performance optimization, and its performance stability is insufficient, making it difficult to meet the needs of environmental protection and sustainable development.
Bio-based aspartic acid ester resin, bio-based isocyanate prepolymer and other materials are used in combination with modified hollow glass microspheres and compounded matte silica to prepare bio-based aspartic polyurea caulking agent. The caulking agent with excellent performance is formed through ring-opening reaction and fusion process.
The prepared caulking agent has good matteness, weather resistance, antibacterial and mildew resistance, and adhesion. The material is safe, the VOC emission is low, the construction is convenient, and the aesthetics and stability are improved.
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Figure BDA0004966508140000081 
Figure BDA0004966508140000091
Abstract
Description
Technical Field
[0001] The present application relates to the field of bio-based caulking agent technology, and in particular to a bio-based aspartame polyurea caulking agent and a preparation method thereof. Background Art
[0002] Asparagus polyurea caulking agent is renowned for its exceptional durability, maintaining its beauty and durability over time. Even in direct sunlight areas such as balconies, indoors, and outdoors, it maintains its vibrant color year-round. Its excellent antioxidant and UV resistance ensures the stability of the product's yellowing resistance. Furthermore, asparagus polyurea caulking agent offers exceptional wear resistance, anti-slip properties, dust resistance, water resistance, moisture resistance, and flame retardancy, effectively resisting various stains and contaminants, keeping floor crevices clean and beautiful. Asparagus polyurea caulking agent is easy to apply, cures quickly, and does not impact construction schedules, greatly facilitating home renovations and construction projects.
[0003] With the global emphasis on environmental protection and sustainable development, market demand for bio-based materials continues to grow. Bio-based caulking agents are poised to become mainstream in the caulking agent market, not only aligning with the global trend toward low-carbon environmental protection but also meeting consumer demand for healthy, safe, and sustainable decoration materials. Bio-based asparagus polyurea caulking agents not only offer excellent color stability and weather resistance, but also boast improved adhesion and higher mechanical strength. However, as a new material, the technology behind bio-based asparagus polyurea caulking agents is not yet fully mature, requiring further research and improvement in production processes, formulation adjustments, and performance optimization. Furthermore, performance stability is limited, requiring further research and improvement. Summary of the Invention
[0004] In order to provide a bio-based polyurea caulking agent product with excellent performance and stability, the present application provides a bio-based asparagus polyurea caulking agent and a preparation method thereof.
[0005] The present application provides a bio-based aspartame polyurea caulking agent, which adopts the following technical solution:
[0006] A bio-based aspartame polyurea seam beautifying agent and a preparation method thereof, wherein the seam beautifying agent comprises component A and component B;
[0007] Component A comprises, by mass, 70-80 parts of bio-based polyaspartic acid ester resin, 2-5 parts of polyurethane resin, 1-3 parts of epoxy acrylate resin, 0-1.5 parts of dispersant, 0-1.5 parts of defoaming agent, 7-12 parts of compounded matte silica, 6-8 parts of hydrophobic fumed silica, 5-8 parts of modified hollow glass microspheres, and 3-7 parts of color paste.
[0008] Calculated by mass, the component B includes: 40-60 parts of bio-based isocyanate prepolymer, 15-30 parts of HDI trimer, 3-8 parts of diaminodicyclohexylmethane, 10-20 parts of isophorone diamine, 3-8 parts of coupling agent, 2-5 parts of hydrophobic fumed silica, and 3-10 parts of modified hollow glass microspheres.
[0009] By adopting the above technical solution, the present application uses bio-based polyaspartic acid ester resin, bio-based isocyanate prepolymer and other materials as the basis to prepare a bio-based aspartic acid polyurea caulking agent. The caulking agent product has good matteness, and the modified hollow glass microspheres added in the fusion form the texture of natural sand. It has excellent weather resistance, antibacterial and mildew resistance, and will not turn yellow. At the same time, it has good adhesion, low viscosity, low resistance, and is easy to construct. The material composition is safe, the VOC emissions are low, and it is environmentally friendly and green.
[0010] Preferably, the coupling agent is a 560 coupling agent.
[0011] Preferably, the dispersant is BYK-2155 dispersant.
[0012] Preferably, the defoaming agent is Digo 900 defoaming agent.
[0013] Preferably, the compound matte silica raw material comprises, by mass percentage, 15-20% Tosoh SS20 matte silica, 20-25% Grace ED40 matte silica, 15-20% Evonik TS100 matte silica, and 35%-50% Aerospaceside 530L matte silica.
[0014] By adopting the above technical solution and the compounded matting silica, not only the fineness and uniformity of the caulking agent are effectively improved, but also a strong matting performance is produced, so that the bio-based aspartame polyurea caulking agent obtains the best matte while ensuring the stability of other properties, effectively improving the aesthetics of the bio-based aspartame polyurea caulking agent, and the compounded matting silica in this application can also enhance the adhesion and stability between the caulking agent and the substrate.
[0015] Preferably, the bio-based polyaspartic acid ester resin is prepared from the following raw materials in parts by weight: 90-110 parts of maleic anhydride, 45-55 parts of bioethanol, 0.09-0.11 parts of boron trifluoride etherate, 345-395 parts of glycidyl ester, 100-120 parts of
[0016] Cyclohexylamine.
[0017] Preferably, the glycidyl ester is one of epoxidized castor oil and epoxidized cottonseed oil.
[0018] Preferably, the bio-based isocyanate prepolymer is a bio-based pentamethylene polyisocyanate prepolymer; the bio-based pentamethylene polyisocyanate prepolymer is prepared from the following raw materials in parts by weight: 100-150 parts of pentamethylene diisocyanate monomer, 0.6-1 parts of antioxidant, 0.1-0.2 parts of catalyst TMR-2, and 0.01-0.02 parts of dibutyl phosphate.
[0019] Preferably, the modified hollow glass microsphere raw material includes alkali-treated hollow glass microspheres and chitosan acetic acid solution with a concentration of 1-5 g / L, and the solid-liquid ratio of the two is 1:8-14 g / mL.
[0020] This application also provides a method for preparing a bio-based aspartame polyurea seam beautifying agent, which adopts the following technical solution:
[0021] A method for preparing a bio-based aspartame polyurea seam beautifying agent comprises the following steps:
[0022] After grafting 70-80 parts of bio-based polyaspartic acid ester resin with 1-3 parts of epoxy acrylate resin by mass, 2-5 parts of polyurethane resin are added and fused. During the fusion process, 0-1.5 parts of dispersant, 0-1.5 parts of defoaming agent, 7-12 parts of compound matte silica, 6-8 parts of hydrophobic fumed silica, 5-8 parts of modified hollow glass microspheres, and 3-7 parts of color paste are added. After uniform fusion, the component A is obtained;
[0023] Component A is mixed with 40-60 parts of bio-based isocyanate prepolymer for a ring-opening reaction. During the reaction, 15-30 parts of HDI trimer, 3-8 parts of diaminodicyclohexylmethane, 10-20 parts of isophoronediamine, 3-8 parts of coupling agent, and 2-5 parts of hydrophobic fumed silica are added. After the reaction, 3-10 parts of modified hollow glass microspheres are added and mixed evenly to obtain the seam beautifying agent product.
[0024] Preferably, the preparation method of the bio-based polyaspartic acid ester resin comprises the following steps:
[0025] After stirring and heating 90-110 parts of maleic anhydride to 60-70°C, 45-55 parts of bioethanol are added dropwise, and the mixture is reacted for 0.5-3 hours to obtain a maleic acid monoester; 0.09-0.11 parts of boron trifluoride etherate are added to the obtained maleic acid monoester and mixed uniformly, and then 345-395 parts of glycidyl ester are added and mixed, and then the mixture is reacted at 80-120°C for 6-24 hours to obtain a modified maleate; 100-120 parts of cyclohexylamine are added dropwise to the modified maleate, and the mixture is reacted at 60-80°C for 10-20 hours after the addition is completed, and then vacuum is applied to obtain a bio-based polyaspartic acid ester resin.
[0026] Preferably, 100-150 parts of pentamethylene diisocyanate monomer and 0.6-1 part of antioxidant are mixed, and nitrogen is purged at 50-60° C. for 10-15 minutes. Then, 0.1-0.2 parts of catalyst TMR-2 are added and reacted for 1-2 hours, and then 0.01-0.02 parts of dibutyl phosphate are added to terminate the reaction to obtain a bio-based isocyanate prepolymer.
[0027] In summary, this application includes at least one of the following beneficial technical effects:
[0028] 1. This application uses bio-based polyaspartic acid ester resin, bio-based isocyanate prepolymer and other materials as the basis to prepare the bio-based aspartic acid polyurea caulking agent. The caulking agent has a good matte finish and is fused with modified hollow glass microspheres to create a natural sand texture. It also has excellent weather resistance, antibacterial and mildew resistance, and does not yellow. It also has good adhesion, low viscosity, low resistance, and is easy to apply. The material ingredients are safe, VOC emissions are low, and it is environmentally friendly and green.
[0029] 2. The compounded matte silica used in this application not only effectively improves the fineness and uniformity of the caulking agent, but also produces a strong matte performance, so that the bio-based asparagine polyurea caulking agent achieves the best matte while ensuring the stability of other properties, effectively improving the aesthetics of the bio-based asparagine polyurea caulking agent. In addition, the compounded matte silica in this application can also enhance the adhesion and stability between the caulking agent and the substrate. DETAILED DESCRIPTION
[0030] The present application is further described in detail below with reference to the embodiments.
[0031] Preparation Example
[0032] Preparation Example 1 Preparation of bio-based polyaspartic acid ester resin
[0033] Preparation Example 1.1
[0034] After stirring and heating 90 g of maleic anhydride to 60°C, 45 g of bioethanol was added dropwise, and the mixture was reacted for 0.5 h to obtain maleic acid monoester; 0.09 g of boron trifluoride etherate was added to the obtained maleic acid monoester and mixed evenly, and then 345 g of epoxy castor oil was added and mixed, and then the mixture was reacted at 80°C for 6 h to obtain modified maleate; 100 g of cyclohexylamine was added dropwise to the modified maleate, and the mixture was reacted at 60°C for 10 h after the addition was completed, and then vacuumed to obtain a bio-based polyaspartic acid ester resin.
[0035] Preparation Example 1.2
[0036] After stirring and heating 100 g of maleic anhydride to 65°C, 50 g of bioethanol was added dropwise, and the mixture was reacted for 2 h to obtain maleic acid monoester; 0.1 g of boron trifluoride etherate was added to the obtained maleic acid monoester and mixed evenly, and then 370 g of epoxy castor oil was added and mixed, and then the mixture was reacted at 100°C for 15 h to obtain modified maleate; 110 g of cyclohexylamine was added dropwise to the modified maleate, and the mixture was reacted at 70°C for 15 h after the addition was completed, and then vacuumed to obtain a bio-based polyaspartic acid ester resin.
[0037] Preparation Example 1.3
[0038] After 110 g of maleic anhydride was stirred and heated to 70°C, 55 g of bioethanol was added dropwise, and the mixture was reacted for 3 hours to obtain maleic acid monoester; 0.11 g of boron trifluoride etherate was added to the obtained maleic acid monoester and mixed evenly, and then 395 g of epoxy castor oil was added and mixed, and then the mixture was reacted at 120°C for 24 hours to obtain modified maleate, 120 g of cyclohexylamine was added dropwise to the modified maleate, and the mixture was reacted at 80°C for 20 hours after the addition was completed, and then vacuumed to obtain a bio-based polyaspartic acid ester resin.
[0039] Preparation Example 1.4
[0040] After stirring and heating 90 g of maleic anhydride to 60°C, 45 g of bioethanol was added dropwise, and the mixture was reacted for 0.5 h to obtain maleic acid monoester; 0.09 g of boron trifluoride etherate was added to the obtained maleic acid monoester and mixed evenly, and then 345 g of epoxy cottonseed oil was added and mixed, and then the mixture was reacted at 80°C for 6 h to obtain modified maleate; 100 g of cyclohexylamine was added dropwise to the modified maleate, and the mixture was reacted at 60°C for 10 h after the addition was completed, and then vacuumed to obtain a bio-based polyaspartic acid ester resin.
[0041] Preparation Example 2 Preparation of bio-based isocyanate prepolymer
[0042] Preparation Example 2.1
[0043] 100 g of pentamethylene diisocyanate monomer, 0.25 g of antioxidant 168, and 0.35 g of antioxidant 1010 were mixed and purged with nitrogen at 50°C for 10 min. Subsequently, 0.1 g of catalyst TMR-2 was added and reacted for 1 h. Then, 0.01 g of dibutyl phosphate was added to terminate the reaction to obtain a bio-based isocyanate prepolymer.
[0044] Preparation Example 2.2
[0045] 125 g of pentamethylene diisocyanate monomer, 0.35 g of antioxidant 168, and 0.45 g of antioxidant 1010 were mixed and purged with nitrogen at 55°C for 12 min. Subsequently, 0.15 g of catalyst TMR-2 was added and reacted for 1.5 h. Then, 0.015 g of dibutyl phosphate was added to terminate the reaction to obtain a bio-based isocyanate prepolymer.
[0046] Preparation Example 2.3
[0047] 150 g of pentamethylene diisocyanate monomer, 0.45 g of antioxidant 168, and 0.55 g of antioxidant 1010 were mixed and purged with nitrogen at 60°C for 15 min. Subsequently, 0.2 g of catalyst TMR-2 was added and reacted for 2 h. Then, 0.02 g of dibutyl phosphate was added to terminate the reaction to obtain a bio-based isocyanate prepolymer.
[0048] Preparation Example 3 Preparation of modified hollow glass microspheres
[0049] Preparation Example 3.1
[0050] S1. 5g of hollow glass microspheres were added to 40g of a 30% sodium hydroxide solution by mass, stirred for 1h, the filtrate was removed by filtration, and the solid was washed several times with deionized water to obtain alkali-treated hollow glass microspheres;
[0051] S2: adding low-viscosity chitosan to the acetic acid solution and stirring evenly to prepare a chitosan acetic acid solution with a concentration of 5 g / L;
[0052] S3. Alkali-treated hollow glass microspheres were added to a chitosan acetic acid solution at a solid-liquid ratio of 1:8 g / mL. After mixing and stirring for 30 minutes, the pH value of the mixture was adjusted to 6 and stirring was continued for 20 minutes to solidify the chitosan molecules adsorbed on the surface of the hollow glass microspheres, forming a dense chitosan deposition film to obtain modified hollow glass microspheres.
[0053] Preparation Example 3.2
[0054] S1. 10g of hollow glass microspheres were added to 60g of a 30% sodium hydroxide solution by mass, stirred for 1.5h, the filtrate was removed by filtration, and the solid was washed several times with deionized water to obtain alkali-treated hollow glass microspheres;
[0055] S2: adding low-viscosity chitosan to the acetic acid solution and stirring evenly to prepare a chitosan acetic acid solution with a concentration of 3 g / L;
[0056] S3. Alkali-treated hollow glass microspheres were added to a chitosan acetic acid solution at a solid-liquid ratio of 1:11 g / mL. After mixing and stirring for 60 minutes, the pH value of the mixture was adjusted to 8 and stirring was continued for 30 minutes to solidify the chitosan molecules adsorbed on the surface of the hollow glass microspheres, forming a dense chitosan deposition film to obtain modified hollow glass microspheres.
[0057] Preparation Example 3.3
[0058] S1. 15g of hollow glass microspheres were added to 80g of 30% sodium hydroxide solution by mass, stirred for 2h, the filtrate was removed by filtration, and the solid was washed several times with deionized water to obtain alkali-treated hollow glass microspheres;
[0059] S2: adding low-viscosity chitosan to the acetic acid solution and stirring evenly to prepare a chitosan acetic acid solution with a concentration of 1 g / L;
[0060] S3. Alkali-treated hollow glass microspheres were added to a chitosan acetic acid solution at a solid-liquid ratio of 1:14 g / mL. After mixing and stirring for 90 minutes, the pH value of the mixture was adjusted to 10 and stirring was continued for 40 minutes to solidify the chitosan molecules adsorbed on the surface of the hollow glass microspheres, forming a dense chitosan deposition film to obtain modified hollow glass microspheres.
[0061] Example
[0062] Example 1
[0063] The coupling agent used in this embodiment is a 560 coupling agent; the compounded matte silica raw material used includes 15% Tosoh SS20 matte silica, 20% Grace ED40 matte silica, 15% Evonik TS100 matte silica, and 50% Aerospaceside 530L matte silica; the bio-based polyaspartic acid ester resin used is from Preparation Example 1.1; the bio-based isocyanate prepolymer used is from Preparation Example 2.1; and the modified hollow glass microspheres used are from Preparation Example 3.1.
[0064] S1. After 70g of bio-based polyaspartic acid ester resin was grafted with 1g of epoxy acrylate resin, 2g of polyurethane resin was added for fusion. During the fusion process, 7g of compound matte silica, 6g of hydrophobic fumed silica, 5g of modified hollow glass microspheres, and 3g of color paste were added. After fusion, the A component was obtained;
[0065] S2. Component A was mixed with 40 g of a bio-based isocyanate prepolymer for a ring-opening reaction. During the reaction, 15 g of HDI trimer, 3 g of diaminodicyclohexylmethane, 10 g of isophoronediamine, 3 g of a 560 coupling agent, and 2 g of hydrophobic fumed silica were added. After the reaction, 3 g of modified hollow glass microspheres were added and mixed evenly to obtain the caulking agent product.
[0066] Example 2
[0067] The dispersant used in this embodiment is BYK-2155 dispersant; the defoamer used is Digo 900 defoamer; the coupling agent used is 560 coupling agent; the compounded matting silica raw material used includes 15% Tosoh SS20 matting silica, 20% Grace ED40 matting silica, 15% Evonik TS100 matting silica, and 50% Aerospace Side 530L matting silica; the bio-based polyaspartic acid ester resin used is from Preparation Example 1.1; the bio-based isocyanate prepolymer used is from Preparation Example 2.1; and the modified hollow glass microspheres used are from Preparation Example 3.1.
[0068] S1. After 75g of bio-based polyaspartic acid resin was grafted with 2g of epoxy acrylate resin, 3.5g of polyurethane resin was added for fusion. During the fusion process, 1g of BYK-2155 dispersant, 1g of Digo 900 defoamer, 9.5g of compound matte silica, 7g of hydrophobic fumed silica, 6.5g of modified hollow glass microspheres, and 5g of color paste were added. After fusion, component A was obtained;
[0069] S2. Component A was mixed with 50 g of a bio-based isocyanate prepolymer for a ring-opening reaction. During the reaction, 22 g of HDI trimer, 5.5 g of diaminodicyclohexylmethane, 15 g of isophorone diamine, 5.5 g of a 560 coupling agent, and 3.5 g of hydrophobic fumed silica were added. After the reaction, 6.5 g of modified hollow glass microspheres were added and mixed evenly to obtain the caulking agent product.
[0070] Example 3
[0071] The dispersant used in this embodiment is BYK-2155 dispersant; the defoamer used is Digo 900 defoamer; the coupling agent used is 560 coupling agent; the compounded matting silica raw material used includes 15% Tosoh SS20 matting silica, 20% Grace ED40 matting silica, 15% Evonik TS100 matting silica, and 50% Aerospace Side 530L matting silica; the bio-based polyaspartic acid ester resin used is from Preparation Example 1.1; the bio-based isocyanate prepolymer used is from Preparation Example 2.1; and the modified hollow glass microspheres used are from Preparation Example 3.1.
[0072] S1. After 80g of bio-based polyaspartic acid ester resin was grafted with 3g of epoxy acrylate resin, 5g of polyurethane resin was added for fusion, and 1.5g of BYK-2155 dispersant, 1.5g of Digo 900 defoamer, 12g of compound matte silica, 8g of hydrophobic fumed silica, 8g of modified hollow glass microspheres, 7g of color paste were added during the fusion process to obtain the A component;
[0073] S2. Component A was mixed with 60 g of a bio-based isocyanate prepolymer for a ring-opening reaction. During the reaction, 30 g of HDI trimer, 8 g of diaminodicyclohexylmethane, 20 g of isophoronediamine, 8 g of a 560 coupling agent, and 5 g of hydrophobic fumed silica were added. After the reaction, 10 g of modified hollow glass microspheres were added and mixed evenly to obtain the caulking agent product.
[0074] Example 4
[0075] The difference between Example 4 and Example 1 is that the bio-based polyaspartic acid ester resin used in Example 4 comes from Preparation Example 1.2.
[0076] Example 5
[0077] The difference between Example 5 and Example 1 is that the bio-based polyaspartic acid ester resin used in Example 5 comes from Preparation Example 1.3.
[0078] Example 6
[0079] The difference between Example 6 and Example 1 is that the bio-based polyaspartic acid ester resin used in Example 6 comes from Preparation Example 1.4.
[0080] Example 7
[0081] The difference between Example 7 and Example 1 is that the bio-based isocyanate prepolymer used in Example 7 comes from Preparation Example 2.2.
[0082] Example 8
[0083] The difference between Example 8 and Example 1 is that the bio-based isocyanate prepolymer used in Example 8 comes from Preparation Example 2.3.
[0084] Example 9
[0085] The difference between Example 9 and Example 1 is that the modified hollow glass microspheres used in Example 9 are all from Preparation Example 3.2.
[0086] Example 10
[0087] The difference between Example 10 and Example 1 is that the modified hollow glass microspheres used in Example 10 are all from Preparation Example 3.3.
[0088] Example 11
[0089] The difference between Example 11 and Example 1 is that the compound matte silica raw material used in Example 11 includes 20% Tosoh SS20 matte silica, 25% Grace ED40 matte silica, 20% Evonik TS100 matte silica, and 35% Aerospace Side 530L matte silica.
[0090] Example 12
[0091] The difference between Example 12 and Example 1 is that the compound matte silica raw material used in Example 12 includes 17% Tosoh SS20 matte silica, 23% Grace ED40 matte silica, 18% Evonik TS100 matte silica, and 42% Aerospace 530L matte silica.
[0092] Comparative Example
[0093] Comparative Example 1
[0094] The difference between Comparative Example 1 and Example 1 is that the hollow glass microspheres used in Comparative Example 1 are unmodified hollow glass microspheres.
[0095] Comparative Example 2
[0096] The difference between Comparative Example 2 and Example 1 is that the matt silica used in Comparative Example 2 is single matt silica, and the model is Aerospace Side 530L matt silica.
[0097] Performance testing
[0098] 1. The caulking agents of Examples 1-12 and Comparative Examples 1-2 were tested for appearance, texture, bonding strength, and surface drying time according to the Q / SY YHF 0099-2021 standard;
[0099] 2. Test the glossiness using the gloss meter of Shenzhen Threentimes Technology Co., Ltd. according to T / CBMF 166-2022 standard;
[0100] 3. Color difference values were tested according to T / CBMF 166-2022 using an array spectrophotometer from Shenzhen Threentime Technology Co., Ltd. 4. Antibacterial rate tests were conducted in accordance with GB / T1741-2007, Determination of Fungal Resistance of Paint Films.
[0101] The results are shown in Table 1.
[0102] The specific test results are as follows:
[0103] Table 1 Performance test results
[0104]
[0105]
[0106] It can be seen from the test results in Table 1 that the bio-based aspartame polyurea caulking agent and its preparation method provided in this application have good matteness, UV resistance, bonding strength, surface drying time, flame retardancy and antibacterial rate. The product has good performance and is easy to construct.
[0107] This specific embodiment is merely an explanation of the present application and is not a limitation of the present application. After reading this specification, those skilled in the art may make non-creative modifications to the present embodiment as needed, but as long as they are within the scope of the claims of the present application, they are protected by the patent law.
Claims
1. A bio-based aspartame polyurea seam beautifying agent, characterized by: The seam beautifying agent includes component A and component B; Calculated by weight, the component A includes: 70-80 parts of bio-based polyaspartic acid ester resin, 2-5 parts of polyurethane resin, 1-3 parts of epoxy acrylate resin, 0-1.5 parts of dispersant, 0-1.5 parts of defoaming agent, 7-12 parts of compounded matte silica, 6-8 parts of hydrophobic fumed silica, 5-8 parts of modified hollow glass microspheres, and 3-7 parts of color paste; The bio-based polyaspartic acid ester resin is prepared from the following raw materials in parts by weight: 90-110 parts of maleic anhydride, 45-55 parts of bioethanol, 0.09-0.11 parts of boron trifluoride etherate, 345-395 parts of glycidyl ester, and 100-120 parts of cyclohexylamine; Calculated by mass, the B component includes: 40-60 parts of bio-based isocyanate prepolymer, 15-30 parts of HDI trimer, 3-8 parts of diaminodicyclohexylmethane, 10-20 parts of isophorone diamine, 3-8 parts of coupling agent, 2-5 parts of hydrophobic fumed silica, and 3-10 parts of modified hollow glass microspheres; The preparation method of the modified hollow glass microspheres is as follows: S1. 10 g of hollow glass microspheres were added to 60 g of a 30% sodium hydroxide solution by mass, stirred for 1.5 h, the filtrate was removed by filtration, and the solid was washed several times with deionized water to obtain alkali-treated hollow glass microspheres; S2. The low viscosity chitosan was added to the acetic acid solution and stirred to prepare a chitosan acetic acid solution having a concentration of 3g / L; S3. Add the alkali-treated hollow glass microspheres to the chitosan acetic acid solution at a solid-liquid ratio of 1:11 g / mL. After mixing and stirring for 60 minutes, adjust the pH value of the mixture to 8 and continue stirring for 30 minutes to allow the chitosan molecules adsorbed on the surface of the hollow glass microspheres to solidify and form a dense chitosan deposition film, thereby obtaining modified hollow glass microspheres.
2. The bio-based aspartame polyurea seam beautifying agent according to claim 1, characterized in that: The coupling agent is KH-560.
3. The bio-based aspartame polyurea seam beautifying agent according to claim 1, characterized in that: The compound matte silica raw material includes, by mass percentage, 15-20% of Tosoh SS20 matte silica, 20-25% of Grace ED40 matte silica, 15-20% of Evonik TS100 matte silica, and 35%-50% of Aerospaceside 530L matte silica.
4. The bio-based aspartame polyurea seam beautifying agent according to claim 1, characterized in that: Glycidyl ester is one of the epoxidized castor oil and epoxidized cottonseed oil.
5. The bio-based aspartame polyurea seam beautifying agent according to claim 1, characterized in that: The bio-based isocyanate prepolymer is a bio-based pentamethylene polyisocyanate prepolymer; the bio-based pentamethylene polyisocyanate prepolymer is prepared from the following raw materials in parts by weight: 100-150 parts of pentamethylene diisocyanate monomer, 0.6-1 parts of antioxidant, 0.1-0.2 parts of TMR-2 catalyst, and 0.01-0.02 parts of dibutyl phosphate.
6. The method for preparing a bio-based aspartame polyurea seam sealant according to claims 1-5, characterized in that: The following steps are involved: After grafting 70-80 parts of bio-based polyaspartic acid ester resin with 1-3 parts of epoxy acrylate resin by mass, 2-5 parts of polyurethane resin are added and blended. During the blending process, 0-1.5 parts of dispersant, 0-1.5 parts of defoaming agent, 7-12 parts of compound matte silica, 6-8 parts of hydrophobic fumed silica, 5-8 parts of modified hollow glass microspheres, and 3-7 parts of color paste are added. After uniform blending, component A is obtained; Component A is mixed with 40-60 parts of bio-based isocyanate prepolymer for a ring-opening reaction. During the reaction, 15-30 parts of HDI trimer, 3-8 parts of diaminodicyclohexylmethane, 10-20 parts of isophoronediamine, 3-8 parts of coupling agent, and 2-5 parts of hydrophobic fumed silica are added. After the reaction, 3-10 parts of modified hollow glass microspheres are added and mixed evenly to obtain the seam beautifying agent product.
7. The method for preparing a bio-based aspartame polyurea seam sealant according to claim 6, characterized in that: The preparation method of the bio-based polyaspartic acid ester resin comprises the following steps: After stirring and heating 90-110 parts of maleic anhydride to 60-70°C, 45-55 parts of bioethanol are added dropwise, and the mixture is reacted for 0.5-3 hours to obtain a maleic acid monoester; 0.09-0.11 parts of boron trifluoride etherate are added to the obtained maleic acid monoester and mixed uniformly, and then 345-395 parts of glycidyl ester are added and mixed, and then the mixture is reacted at 80-120°C for 6-24 hours to obtain a modified maleate; 100-120 parts of cyclohexylamine are added dropwise to the modified maleate, and the mixture is reacted at 60-80°C for 10-20 hours after the addition is completed, and then vacuum is applied to obtain a bio-based polyaspartic acid ester resin.
8. The method for preparing a bio-based aspartame polyurea seam beautifying agent according to claim 6, characterized in that: The preparation method of the bio-based isocyanate prepolymer comprises the following steps: After mixing 100-150 parts of pentamethylene diisocyanate monomer and 0.6-1 part of antioxidant, nitrogen is purged at 50-60°C for 10-15 minutes, and then 0.1-0.2 parts of TMR-2 catalyst are added to react for 1-2 hours, and then 0.01-0.02 parts of dibutyl phosphate are added to terminate the reaction to obtain a bio-based isocyanate prepolymer.
Citation Information
Patent Citations
Printing ink for gold stamping transfer and preparation method thereof
CN116445033A
Polyaspartic acid ester resin and preparation method thereof
CN116891445A
Matt color sand polyurea sealant
CN117004303A
Preparation method of bio-based blocked isocyanate cross-linking agent
CN117264161A