New method for preparing polyurea sealant ceramic adhesive
Patent Information
- Application Number
- CN202611340219.5
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2026-09-01
- Publication Date
- 2026-10-27
AI Technical Summary
[0003]其一，固化速度过快导致操作窗口极窄
[0016]采用本发明提供的技术方案，与已知的公有技术相比，具有如下有益效果：
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Figure CN122978901A_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the fields of building decoration adhesives and polymer functional materials, specifically to a new method for preparing polyurea grout sealant. Background Technology
[0002] Currently, the mainstream grouting products on the market are mainly epoxy resin-based sealants. Although they possess high hardness and adhesion, they have inherent defects in yellowing resistance and water resistance, especially prone to yellowing and whitening under ultraviolet radiation and humid environments. To overcome the shortcomings of epoxy sealants, polyurea sealants have gradually become a research hotspot in the industry. Existing polyurea sealants typically use polyaspartic acid esters and isocyanate components for curing. While significant progress has been made in yellowing resistance and water resistance, many technical challenges still need to be addressed.
[0003] Firstly, the excessively fast curing speed results in a very narrow working window. The amine groups in existing conventional polyurea grout have extremely high reactivity with isocyanates, and the edge-pressing time is typically only a few minutes. This leaves insufficient time for workers to press the grout lines, requiring two people to work together, significantly increasing labor costs and limiting its widespread adoption in the home improvement market. Secondly, it has a pungent odor and poor environmental performance. Some existing polyurea grouts contain unreacted amine monomers remaining from the synthesis process, or contain solvents such as benzyl alcohol and large amounts of odor masking agents to adjust rheology and solubility, resulting in a pungent odor during construction, failing to meet the stringent green and environmentally friendly requirements of modern families. Thirdly, it is difficult to balance flexibility and adhesion. Existing polyurea systems have a high cross-linking density after curing, leading to a brittle material with insufficient flexibility, making it prone to cracking when exposed to the thermal expansion and contraction of tiles. Simultaneously, some polyurea materials have poor adhesion to the tile joint interface, easily leading to edge detachment after long-term use. Fourthly, it has poor storage stability. The isocyanate component in polyurea grout is extremely sensitive to moisture. If the existing formula uses hydrophilic silicone containing hydroxyl groups or has an improper waterproof design, it is very easy to absorb moisture from the air during storage, which can cause the product to swell or prematurely cure and fail, seriously affecting the product's shelf life and construction performance. Summary of the Invention
[0004] To achieve the above objectives, the present invention aims to provide a novel method for preparing polyurea grout sealant, specifically addressing the issues of yellowing resistance and water resistance in the aforementioned product. The method includes the following steps: S1. Synthesis of modified polyurethane: First, isophorone diisocyanate (IPDI) and hexamethylene diisocyanate (HDI) are modified with polycaprolactone polyol 220 under the catalysis of dibutyltin dilaurate and the action of polyurethane (PU) dehydrating agent BF-5. Then, hexamethylene diisocyanate trimer (HDI trimer) is added and stirred evenly. Finally, hydrogenated cashew nut shell powder is added to further modify the isocyanate. The hydroxyl groups of hydrogenated cashew nut shell powder consume part of the -NCO to reduce its activity, thus obtaining the modified polyurethane. S2. Preparation of polyurethane component: Modified polyurethane, hydrophobic fumed silica, toughening agent diisononyl cyclohexane 1,2-dicarboxylate, and waterproofing agent 3A activated powder molecular sieve are added to a high-speed dispersion device, and the polyurethane component is obtained by high-speed dispersion under vacuum. S3. Synthesis of modified amine resin: First, N,N'-bis(3-aminopropyl)-ethylenediamine modified amine and diisooctyl maleate were synthesized under the catalysis of tetramethylammonium hydroxide. Then, N-cyclohexyl-N'-(3-aminopropyl)-1,3-propanediamine modified amine and diisooctyl maleate were synthesized under the catalysis of tetramethylammonium hydroxide. S4. Preparation of amine resin components: N,N'-bis(3-aminopropyl)-ethylenediamine modified amine, N-cyclohexyl-N'-(3-aminopropyl)-1,3-propanediamine modified amine, hydrophobic silica, anti-flow agent, and color paste were added to a high-speed dispersion vessel and dispersed at high speed under vacuum to obtain amine resin components.
[0005] S5. Preparation of polyurea grout tube: Then, the polyurethane component and the amino resin component are injected into the grout tube in equal volumes to obtain the final polyurea grout true porcelain adhesive product.
[0006] Preferably, in step one, the isophorone diisocyanate (IPDI) comprises 15-35 parts, hexamethylene diisocyanate (HDI) comprises 5-15 parts, dibutyltin dilaurate comprises 0.01-0.05 parts, polyurethane (PU) dehydrating agent BF-5 comprises 0.01-0.05 parts, polycaprolactone polyol 220 comprises 30-40 parts, hexamethylene diisocyanate trimer (HDI trimer) comprises 25-35 parts, and hydrogenated cashew nut shell powder comprises 1-5 parts.
[0007] Preferably, in step three, the N,N'-bis(3-aminopropyl)-ethylenediamine modified amine is 17.4 parts, diisooctyl maleate is 68.8-69.8 parts, and tetramethylammonium hydroxide is 0.001-0.005 parts.
[0008] Preferably, in step three, the following components are used: 21.3 parts of N-cyclohexyl-N'-(3-aminopropyl)-1,3-propanediamine, 68.8-69.8 parts of diisooctyl maleate, and 0.001-0.005 parts of tetramethylammonium hydroxide.
[0009] Preferably, in step four, the N,N'-bis(3-aminopropyl)-ethylenediamine modified amine resin is 40-70 parts and the N-cyclohexyl-N'-(3-aminopropyl)-1,3-propanediamine amine resin is 30-60 parts.
[0010] Preferably, in step one, the temperature of the modified polyurethane insulation is controlled at 80-90℃.
[0011] Preferably, in step one, the modified polyurethane catalyst is dibutyltin dilaurate, and the dehydrating agent used is polyurethane (PU) dehydrating agent BF-5.
[0012] Preferably, in step three, the catalyst for the modified amine resin synthesis reaction is tetramethylammonium hydroxide.
[0013] Preferably, in step one, the insulation temperature of the amine resin is controlled at 80-90℃.
[0014] Preferably, in step two, the polyurethane component uses hydrophobic fumed silica, the toughening agent is diisononyl cyclohexane-1,2-dicarboxylate, and the waterproofing agent is 3A activated molecular sieve.
[0015] Beneficial effects
[0016] Compared with known public technologies, the technical solution provided by this invention has the following beneficial effects:
[0017] This invention, through the synergistic design of a specific Michael addition-modified amine and hydrogenated cashew phenol-terminated isocyanate, perfectly balances curing speed, flexibility, and hardness, completely eliminates the acidic smell, and achieves excellent water resistance and yellowing resistance, possessing significant industrial application value. The synergistic effect of these features perfectly balances the curing speed, flexibility, and hardness of the grout, completely eliminates the acidic smell of traditional polyurea products, and enables convenient single-person application.
[0018] This invention addresses the issue of storage tube expansion at the source of the chemical formula, ensuring excellent water resistance, yellowing resistance, and long-term storage stability of the product. It completely converts primary amines into secondary amines, significantly reducing the reactivity of amine hydrogens with isocyanate groups, effectively solving the problems of insufficient edge-pressing time and the need for two-person application in traditional products, while also significantly improving the product's flexibility. The use of hydrogenated cashew phenols to gently reduce isocyanate activity further extends the edge-pressing time, synergizing with secondary amine modification, completely eliminating the acidic taste of traditional products and improving the construction environment. By strictly selecting hydrophobic fumed silica and combining it with molecular sieve waterproofing agents, the storage failure problem caused by the reaction of hydroxyl groups in hydrophilic fumed silica with polyurethane is completely avoided, fundamentally ensuring the product's water resistance and storage stability. Attached Figure Description
[0019] Figure 1 Flowchart of the manufacturing process for the polyurea grout sealant of this invention;
[0020] Figure 2 This is a comparison diagram of the yellowing resistance performance of the present invention;
[0021] Figure 3 This is a comparison chart of the tensile strength performance of the present invention. Detailed Implementation
[0022] To enable those skilled in the art to better understand the present invention, the technical solutions of the present invention will be clearly and completely described below with reference to the accompanying drawings of the embodiments of the present invention. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort should fall within the scope of protection of the present invention.
[0023] The following is in conjunction with the appendix Figure 1 , 2 3. The present invention will be described in further detail:
[0024] I. Implementation Examples
[0025] Example 1 (Sample #1):
[0026] Step 1: Synthesis of modified polyurethane: First, 25 parts of isophorone diisocyanate, 10 parts of hexamethylene diisocyanate, 0.03 parts of dibutyltin dilaurate, and 0.03 parts of polyurethane dehydrating agent BF-5 were added to a reactor. The mixture was heated to 85°C under nitrogen protection and reacted for 2 hours. Then, 35 parts of polycaprolactone polyol 220 were added for modification reaction for 1 hour. Next, 30 parts of hexamethylene diisocyanate trimer were added and stirred evenly. Finally, 3 parts of hydrogenated cashew nut shell powder were added to further modify the isocyanate, and the reaction was carried out for 1.5 hours to obtain modified polyurethane.
[0027] Step 2, Preparation of polyurethane component: Add 70 parts of the above modified polyurethane, 3 parts of hydrophobic fumed silica, 15 parts of diisononyl cyclohexane-1,2-dicarboxylate and 2 parts of 3A activated molecular sieve powder to a high-speed dispersion device, and disperse at high speed for 1 hour under a vacuum of -0.09 MPa to obtain the polyurethane component.
[0028] Step 3: Synthesis of modified amine resin: First, 17.4 parts of N,N'-bis(3-aminopropyl)-ethylenediamine (N4 amine) and 69.3 parts of diisooctyl maleate were reacted at 85°C for 3 hours under the catalysis of 0.003 parts of tetramethylammonium hydroxide to synthesize the modified amine; then, 21.3 parts of N-cyclohexyl-N'-(3-aminopropyl)-1,3-propanediamine and 69.3 parts of diisooctyl maleate were reacted at 85°C for 3 hours under the catalysis of 0.003 parts of tetramethylammonium hydroxide to synthesize the modified amine.
[0029] Step 4: Preparation of amine resin component: Add 55 parts of N,N'-bis(3-aminopropyl)-ethylenediamine modified amine, 40 parts of N-cyclohexyl-N'-(3-aminopropyl)-1,3-propanediamine modified amine, 3 parts of hydrophobic fumed silica, 1 part of anti-flow agent and 5 parts of color paste to a high-speed dispersion vessel, and disperse at high speed for 1.5 hours under a vacuum of -0.09 MPa to obtain amine resin component;
[0030] Step 5: Finished Product Preparation: Inject equal volumes of the polyurethane component and the amine resin component into the grout tube to obtain the final polyurea grout sealant product.
[0031] Example 2 (Sample #2):
[0032] Step 1: Add 15 parts of isophorone diisocyanate, 15 parts of hexamethylene diisocyanate, 0.01 parts of dibutyltin dilaurate, and 0.05 parts of polyurethane dehydrating agent BF-5 to the reactor, heat to 80℃, and maintain the temperature for 2.5 hours; add 40 parts of polycaprolactone polyol 220 and react for 1.5 hours; add 25 parts of hexamethylene diisocyanate trimer and stir; finally, add 5 parts of hydrogenated cashew nut shell powder for modification and maintain the temperature for 1 hour.
[0033] Step 2: Add 60 parts of modified polyurethane, 5 parts of hydrophobic fumed silica, 20 parts of diisononyl cyclohexane-1,2-dicarboxylate and 4 parts of 3A activated molecular sieve powder to a high-speed dispersion device, and disperse under vacuum at high speed for 1 hour.
[0034] Step 3: Modified amines were synthesized by reacting 17.4 parts of N,N'-bis(3-aminopropyl)-ethylenediamine and 68.8 parts of diisooctyl maleate at 80°C for 3.5 hours under the catalysis of 0.001 parts of tetramethylammonium hydroxide; modified amines were also synthesized by reacting 21.3 parts of N-cyclohexyl-N'-(3-aminopropyl)-1,3-propanediamine and 69.8 parts of diisooctyl maleate at 80°C for 3.5 hours under the catalysis of 0.005 parts of tetramethylammonium hydroxide.
[0035] Step 4: Add 40 parts of N,N'-bis(3-aminopropyl)-ethylenediamine modified amine, 60 parts of N-cyclohexyl-N'-(3-aminopropyl)-1,3-propanediamine modified amine, 5 parts of hydrophobic fumed silica, 3 parts of anti-flow agent and 8 parts of color paste, and disperse under vacuum at high speed for 1.5 hours;
[0036] Step 5: Mix the two components in equal volumes to obtain the finished product;
[0037] Example 3 (Sample #3):
[0038] Step 1: Add 35 parts of isophorone diisocyanate, 5 parts of hexamethylene diisocyanate, 0.05 parts of dibutyltin dilaurate, and 0.01 parts of polyurethane dehydrating agent BF-5 to the reactor, heat to 90℃, and maintain the temperature for 1.5 hours; add 30 parts of polycaprolactone polyol 220 and react for 1 hour; add 35 parts of hexamethylene diisocyanate trimer and stir; finally, add 1 part of hydrogenated cashew nut shell powder for modification and maintain the temperature for 2 hours.
[0039] Step 2: Add 80 parts modified polyurethane, 2 parts hydrophobic fumed silica, 10 parts diisononyl cyclohexane-1,2-dicarboxylate and 1 part 3A activated molecular sieve powder, and disperse under vacuum at high speed for 1.2 hours.
[0040] Step 3: Modified amines were synthesized by reacting 17.4 parts of N,N'-bis(3-aminopropyl)-ethylenediamine and 69.8 parts of diisooctyl maleate at 90°C for 2.5 hours under the catalysis of 0.005 parts of tetramethylammonium hydroxide; modified amines were also synthesized by reacting 21.3 parts of N-cyclohexyl-N'-(3-aminopropyl)-1,3-propanediamine and 68.8 parts of diisooctyl maleate at 90°C for 2.5 hours under the catalysis of 0.001 parts of tetramethylammonium hydroxide.
[0041] Step 4: Add 70 parts of N,N'-bis(3-aminopropyl)-ethylenediamine modified amine, 30 parts of N-cyclohexyl-N'-(3-aminopropyl)-1,3-propanediamine modified amine, 2 parts of hydrophobic fumed silica, 2 parts of anti-flow agent and 3 parts of color paste, and disperse under vacuum at high speed for 1 hour;
[0042] Step 5: Mix the two components in equal volumes to obtain the finished product;
[0043] Example 4 (Sample #4):
[0044] Step 1: Add 20 parts of isophorone diisocyanate, 12 parts of hexamethylene diisocyanate, 0.02 parts of dibutyltin dilaurate, and 0.04 parts of polyurethane dehydrating agent BF-5 to the reactor, heat to 82℃, and maintain the temperature for 2 hours; add 38 parts of polycaprolactone polyol 220 and react for 1.2 hours; add 28 parts of hexamethylene diisocyanate trimer and stir; finally, add 4 parts of hydrogenated cashew nut shell powder for modification and maintain the temperature for 1.5 hours.
[0045] Step 2: Add 65 parts modified polyurethane, 4 parts hydrophobic fumed silica, 18 parts diisononyl cyclohexane-1,2-dicarboxylate and 3 parts 3A activated molecular sieve powder, and disperse under vacuum at high speed for 1 hour.
[0046] Step 3: Modified amines were synthesized by reacting 17.4 parts of N,N'-bis(3-aminopropyl)-ethylenediamine and 69.0 parts of diisooctyl maleate at 88°C for 3 hours under the catalysis of 0.002 parts of tetramethylammonium hydroxide; modified amines were also synthesized by reacting 21.3 parts of N-cyclohexyl-N'-(3-aminopropyl)-1,3-propanediamine and 69.5 parts of diisooctyl maleate at 88°C for 3 hours under the catalysis of 0.004 parts of tetramethylammonium hydroxide.
[0047] Step 4: Add 45 parts of N,N'-bis(3-aminopropyl)-ethylenediamine modified amine, 55 parts of N-cyclohexyl-N'-(3-aminopropyl)-1,3-propanediamine modified amine, 4 parts of hydrophobic fumed silica, 1.5 parts of anti-flow agent and 6 parts of color paste, and disperse under vacuum at high speed for 1.5 hours;
[0048] Step 5: Mix the two components in equal volumes to obtain the finished product;
[0049] Example 5 (Sample #5):
[0050] Step 1: Add 30 parts of isophorone diisocyanate, 8 parts of hexamethylene diisocyanate, 0.04 parts of dibutyltin dilaurate, and 0.02 parts of polyurethane dehydrating agent BF-5 to the reactor, heat to 88℃, and maintain the temperature for 2.2 hours; add 32 parts of polycaprolactone polyol 220 and react for 1.3 hours; add 32 parts of hexamethylene diisocyanate trimer and stir; finally, add 2 parts of hydrogenated cashew nut shell powder for modification and maintain the temperature for 1.8 hours.
[0051] Step 2: Add 75 parts modified polyurethane, 2.5 parts hydrophobic fumed silica, 14 parts diisononyl cyclohexane-1,2-dicarboxylate and 2.5 parts 3A activated molecular sieve powder, and disperse under vacuum at high speed for 1.1 hours;
[0052] Step 3: Modified amines were synthesized by reacting 17.4 parts of N,N'-bis(3-aminopropyl)-ethylenediamine and 69.5 parts of diisooctyl maleate at 82°C for 3.2 hours under the catalysis of 0.004 parts of tetramethylammonium hydroxide; modified amines were also synthesized by reacting 21.3 parts of N-cyclohexyl-N'-(3-aminopropyl)-1,3-propanediamine and 69.0 parts of diisooctyl maleate at 82°C for 3.2 hours under the catalysis of 0.002 parts of tetramethylammonium hydroxide.
[0053] Step 4: Add 60 parts of N,N'-bis(3-aminopropyl)-ethylenediamine modified amine, 45 parts of N-cyclohexyl-N'-(3-aminopropyl)-1,3-propanediamine modified amine, 3.5 parts of hydrophobic fumed silica, 2.5 parts of anti-flow agent and 10 parts of color paste, and disperse under vacuum at high speed for 1.3 hours;
[0054] Step 5: Mix the two components in equal volumes to obtain the finished product.
[0055] II. Effect Verification
[0056] The testing standards are adjusted based on GB / T 14683-2017 Silicone and Modified Silicone Building Sealants and JC / T 801-2019 National Standard for Polyurethane Building Sealants. The main tests are surface drying time, tensile strength, elongation at break and resistance to yellowing.
[0057] Test data show that the polyurea grout prepared in Examples 1 to 5 exhibit excellent overall performance in terms of surface drying time, mechanical properties, and resistance to yellowing. This is attributed to the introduction of hydrogenated cashew phenol into the modified polyurethane, which effectively reduces the activity of isocyanate, improves the storage stability of the system, and enhances the yellowing resistance of the final product. Simultaneously, the synergistic effect of the two modified amine resins ensures rapid curing and excellent flexibility of the product.
[0058] Table 1: Main performance tests of the embodiments.
[0059] Example 1 2.5 15.2 120 0.8 Example 2 2.3 14.8 115 0,9 Example 3 2.4 15.0 130 0.8 Example 4 2.6 14.5 125 1.0 Example 5 2.2 15.5 118 0.7
[0060] III. Application Scenarios
[0061] (a) Interior beautification with high-end building materials
[0062] The polyurea grout prepared using this technical solution possesses excellent waterproof, mildew-proof, yellowing-resistant, and high tensile strength properties, making it widely applicable for beautifying and protecting the gaps in high-end indoor ceramic tiles, marble, slabs, and other building materials. Its delicate texture and rich color selection perfectly match various high-end interior design styles.
[0063] (II) Special Environmental Protection
[0064] Especially in damp environments such as kitchens and bathrooms, as well as areas with strong ultraviolet radiation such as balconies and sunrooms, this product can maintain its vibrant color for a long time without shrinking or cracking. Its superior hydrophobicity and molecular sieve waterproof technology effectively prevent the penetration of moisture and stains, completely solving the industry pain points of traditional grout sealants, such as yellowing, mold growth, and easy peeling.
[0065] IV. Performance Comparison and Verification
[0066] Comparative Example 1 (Sample 6#)
[0067] This comparative example provides a polyurea grout sealant, the preparation method of which is basically the same as that of Example 1, except that the raw material ratios exceed the scope of this invention: the amount of isophorone diisocyanate is 40 parts, which exceeds the range of 15 to 35 parts; the amount of hydrogenated cashew phenol is 0.5 parts, which exceeds the range of 1 to 5 parts; the amount of N,N'-bis(3-aminopropyl)-ethylenediamine modified amine is 20 parts, which exceeds the range of 40 to 70 parts; and the amount of N-cyclohexyl-N'-(3-aminopropyl)-1,3-propanediamine modified amine is 80 parts, which exceeds the range of 30 to 60 parts.
[0068] Comparative Example 2 (Sample 7#)
[0069] This comparative example provides a polyurea grout sealant, the preparation method of which is basically the same as that of Example 1, the difference being the component substitution: commercially available ordinary polyaspartic acid ester resin is used to replace N,N'-bis(3-aminopropyl)-ethylenediamine modified amine and N-cyclohexyl-N'-(3-aminopropyl)-1,3-propanediamine modified amine; at the same time, hydrophilic fumed silica is used to replace hydrophobic fumed silica.
[0070] Comparative Example 3 (Sample 8#)
[0071] This comparative example provides a polyurea grout sealant, the preparation method of which differs from that of Example 1 in the process steps: in the modified polyurethane synthesis step, the step of adding hydrogenated cashew phenol to further cap and deactivate the isocyanate group is omitted, that is, after adding hexamethylene diisocyanate trimer and stirring, the polyurethane component is directly prepared by high-speed dispersion without deactivation treatment.
[0072] Comparative Example 4 (Sample 9#)
[0073] This comparative example uses a common polyaspartic acid ester polyurea grout sealant popular on the market. Its amine resin component consists of common polyaspartic acid ester, hydrophilic silicone, anti-flow agent, and a large amount of odor masking agent; the isocyanate component consists of unmodified hexamethylene diisocyanate trimer and hydrophobic silicone.
[0074] (a) Testing conditions and standards
[0075] To further verify the superiority of the technical solution of the present invention, performance tests were conducted on the polyurea grout prepared in Examples 1 to 5 and Comparative Examples 1 to 4. The tests were conducted at 25 degrees Celsius, and the test standards were adjusted according to GB / T14683-2017 Silicone and Modified Silicone Building Sealants and JC / T 801-2019 Polyurethane Building Sealants national standards. The main parameters examined were surface drying time, tensile strength, and resistance to yellowing.
[0076] (II) Performance Comparison Data
[0077] The tile grouts prepared in Examples 1 to 5 and Comparative Examples 1 to 4 were subjected to performance tests at 25 degrees Celsius. The results are shown in the table below:
[0078] Table 2: Comparative performance test.
[0079] Example 1 Surface drying time 2.5h Example 1 Tensile strength 15.2MPa Example 1 Yellowing resistance 0.8 Example 2 Surface drying time 2.3h Example 2 Tensile strength 14.8MPa Example 2 Yellowing resistance 0.9 Example 3 Surface drying time 2.4h Example 3 Tensile strength 15.0MPa Example 3 Yellowing resistance 0.8 Example 4 Surface drying time 2.6h Example 4 Tensile strength 14.5MPa Example 4 Yellowing resistance 1.0 Example 5 Surface drying time 2.2h Example 5 Tensile strength 15.5MPa Example 5 Yellowing resistance 0.7 Comparative Example 1 Surface drying time 1.2h Comparative Example 1 Tensile strength 9.5MPa Comparative Example 1 Yellowing resistance 2.5 Comparative Example 2 Surface drying time 3.5h Comparative Example 2 Tensile strength 10.2MPa Comparative Example 2 Yellowing resistance 3.1 Comparative Example 3 Surface drying time 0.8h Comparative Example 3 Tensile strength 11.0MPa Comparative Example 3 Yellowing resistance 1.5 Comparative Example 4 Surface drying time 3.0h Comparative Example 4 Tensile strength 12.0MPa Comparative Example 4 Yellowing resistance 2.8
[0080] (III) Analysis of Advantages and Effects
[0081] The comparative data above show that the polyurea grout prepared in Examples 1 to 5 are significantly better than the comparative examples in all performance indicators.
[0082] In Comparative Example 1, the amounts of isophorone diisocyanate, hydrogenated cashew nut shell powder, and the two modified amines exceeded the limits specified in this invention, leading to an imbalance in the reaction system. Although the surface drying time was shortened to 1.2 hours, the tensile strength dropped significantly to 9.5 MPa, and the yellowing resistance deteriorated to 2.5. This indicates that strictly controlling each component within a reasonable range is crucial to ensuring mechanical properties and weather resistance. Comparative Example 2 used ordinary polyaspartic acid ester resin and hydrophilic fumed silica to replace the core modifying components of this invention, resulting in a surface drying time extended to 3.5 hours, a tensile strength reduced to 10.2 MPa, and a yellowing resistance as high as 3.1. This demonstrates that the synergistic effect of the specific modified amine resin and hydrophobic fumed silica of this invention can effectively improve the curing speed and overall mechanical properties. Comparative Example 3 omitted the deactivation modification step of hydrogenated cashew nut shell powder, resulting in excessively high isocyanate activity, an extremely short surface drying time of only 0.8 hours, severely insufficient construction time, and a tensile strength of only 11.0 MPa, as well as poor yellowing resistance. This demonstrates that the deactivation treatment of hydrogenated cashew nut shells plays an irreplaceable role in regulating reaction rates and improving product flexibility and resistance to yellowing.
[0083] In summary, comparing Examples 1 to 5 with Comparative Example 4, it is evident that commercially available similar products are inferior to the embodiments of this invention in terms of surface drying time, tensile strength, and resistance to yellowing. This invention, through a unique two-component modification design and precise process control, achieves superior performance with moderate surface drying time, tensile strength exceeding 14.5 MPa, and a color difference of less than 1.0 in resistance to yellowing, completely solving the industry pain points of traditional products such as easy yellowing and insufficient strength.
[0084] The above embodiments are only used to illustrate the technical solutions of the present invention, and are not intended to limit it. Although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that modifications can still be made to the technical solutions described in the foregoing embodiments, or equivalent substitutions can be made to some of the technical features. Such modifications or substitutions will not cause the essence of the corresponding technical solutions to deviate from the spirit and scope of the technical solutions of the embodiments of the present invention.
Claims
1. A novel method for preparing polyurea grout sealant, characterized in that: Includes the following steps: S1. Synthesis of modified polyurethane: First, isophorone diisocyanate (IPDI) and hexamethylene diisocyanate (HDI) are modified with polycaprolactone polyol 220 under the catalysis of dibutyltin dilaurate and the action of polyurethane (PU) dehydrating agent BF-5. Then, hexamethylene diisocyanate trimer (HDI trimer) is added and stirred evenly. Finally, hydrogenated cashew nut shell powder is added to further modify the isocyanate. The hydroxyl groups of hydrogenated cashew nut shell powder consume part of the -NCO to reduce its activity, thus obtaining the modified polyurethane. S2. Preparation of polyurethane component: Modified polyurethane, hydrophobic fumed silica, toughening agent diisononyl cyclohexane 1,2-dicarboxylate, and waterproofing agent 3A activated powder molecular sieve are added to a high-speed dispersion device, and the polyurethane component is obtained by high-speed dispersion under vacuum. S3. Synthesis of modified amine resin: First, N,N'-bis(3-aminopropyl)-ethylenediamine modified amine and diisooctyl maleate were synthesized under the catalysis of tetramethylammonium hydroxide. Then, N-cyclohexyl-N'-(3-aminopropyl)-1,3-propanediamine modified amine and diisooctyl maleate were synthesized under the catalysis of tetramethylammonium hydroxide. S4. Preparation of amine resin components: N,N'-bis(3-aminopropyl)-ethylenediamine modified amine, N-cyclohexyl-N'-(3-aminopropyl)-1,3-propanediamine modified amine, hydrophobic silica, anti-flow agent, and color paste were added to a high-speed dispersion vessel and dispersed at high speed under vacuum to obtain amine resin components. S5. Preparation of polyurea grout tube: Then, the polyurethane component and the amine resin component are injected into the grout tube in equal volumes to obtain the final polyurea grout true porcelain adhesive product.
2. The novel method for preparing polyurea grout sealant according to claim 1, characterized in that: In step one, the isophorone diisocyanate (IPDI) is 15-35 parts, hexamethylene diisocyanate (HDI) is 5-15 parts, dibutyltin dilaurate is 0.01-0.05 parts, polyurethane (PU) dehydrating agent BF-5 is 0.01-0.05 parts, polycaprolactone polyol 220 is 30-40 parts, hexamethylene diisocyanate trimer (HDI trimer) is 25-35 parts, and hydrogenated cashew nut shell powder is 1-5 parts.
3. The novel method for preparing polyurea grout sealant according to claim 1, characterized in that: In step three, the N,N'-bis(3-aminopropyl)-ethylenediamine modified amine is 17.4 parts, diisooctyl maleate is 68.8-69.8 parts, and tetramethylammonium hydroxide is 0.001-0.005 parts.
4. A novel method for preparing polyurea grout sealant according to claim 1, characterized in that: In step three, the following components are used: 21.3 parts of N-cyclohexyl-N'-(3-aminopropyl)-1,3-propanediamine, 68.8-69.8 parts of diisooctyl maleate, and 0.001-0.005 parts of tetramethylammonium hydroxide.
5. A novel method for preparing polyurea grout sealant according to claim 1, characterized in that: In step four, the N,N'-bis(3-aminopropyl)-ethylenediamine modified amine resin is 40-70 parts and the N-cyclohexyl-N'-(3-aminopropyl)-1,3-propanediamine amine resin is 30-60 parts.
6. A novel method for preparing polyurea grout sealant according to claim 1, characterized in that: In step one, the temperature of the modified polyurethane insulation is controlled at 80-90℃.
7. A novel method for preparing polyurea grout sealant according to claim 1, characterized in that: In step one, the modified polyurethane catalyst is dibutyltin dilaurate, and the dehydrating agent used is polyurethane (PU) dehydrating agent BF-5.
8. A novel method for preparing polyurea grout sealant according to claim 1, characterized in that: In step three, the catalyst for the synthesis reaction of the modified amine resin is tetramethylammonium hydroxide.
9. A novel method for preparing polyurea grout sealant according to claim 1, characterized in that: In step one, the insulation temperature of the amine resin is controlled at 80-90℃.
10. A novel method for preparing polyurea grout sealant according to claim 1, characterized in that: In step two, the polyurethane component uses hydrophobic fumed silica, the toughening agent is diisononyl cyclohexane-1,2-dicarboxylate, and the waterproofing agent is 3A activated molecular sieve.