Water-based organosilicon monomer based on trisulfonic acid group and quaternary ammonium salt modification, preparation method of water-based organosilicon monomer and application of water-based organosilicon monomer in water-based resin

The method for preparing waterborne organosilicon monomers modified with trisulfonic acid groups and quaternary ammonium salts solves the problem of poor water solubility of traditional organosilicon monomers, achieving stable dispersion and performance retention of waterborne organosilicon resins, which is suitable for large-scale production.

CN121758488APending Publication Date: 2026-03-31WUHAN INST OF TECH
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-12-10
Publication Date
2026-03-31

AI Technical Summary

Technical Problem

Traditional organosilicon monomers have poor solubility in water. Existing methods, such as adding surfactants or emulsifiers, have stability issues and affect resin performance, making it difficult to achieve long-term stable water dispersion.

Method used

A waterborne organosilicon monomer modified with trisulfonic acid group and quaternary ammonium salt is prepared by nucleophilic addition reaction, forming a self-emulsifying effect and enhancing molecular polarity and hydration ability. When preparing waterborne organosilicon resin, only a very small amount needs to be added to achieve excellent water dispersibility and storage stability.

Benefits of technology

It achieves stable dispersion of waterborne silicone resin in water, avoids damage to resin performance by surfactants, maintains core properties such as heat resistance and mechanical strength, and has a simple and efficient process suitable for large-scale production.

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Abstract

The invention discloses a water-based organic silicon monomer based on trisulfonic acid group and quaternary ammonium salt modification, a preparation method thereof and application of the water-based organic silicon monomer in water-based resin, and belongs to the field of organic silicon resin. According to the water-based organic silicon monomer, three sulfonic acid groups and one quaternary ammonium salt group are introduced at the same time to generate a synergistic interaction effect, so that the molecular polarity and the hydration capability are remarkably enhanced, and the monomer is endowed with excellent water solubility; when the obtained water-based organic silicon monomer is used for preparing the water-based organic silicon resin, the interface energy of a system can be effectively reduced only by adding a very small amount of the water-based organic silicon monomer, the obtained water-based organic silicon resin realizes excellent dispersion stability, and the inherent hydrophobicity, heat resistance and mechanical property are not influenced after the resin forms a film. The preparation method is simple and efficient, the synthetic route steps are simple, the reaction conditions are mild, and complex post-treatment is not needed; the whole process is high in yield, easy in impurity control, green, environment-friendly and controllable in cost, has good large-scale production potential, and can meet the industrialization requirement of the high-performance water-based additive.
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Description

Technical Field

[0001] This invention belongs to the field of organosilicon resins, specifically relating to a waterborne organosilicon monomer modified with trisulfonic acid group and quaternary ammonium salt, its preparation method, and its application in waterborne resins. Background Technology

[0002] Organosilicon resins, with their excellent comprehensive properties such as high hardness, good weather resistance, good chemical stability, and good electrical insulation, demonstrate core value in many high-tech fields, including construction, medical, aerospace, and industrial applications. Organosilicon monomers are the basic building blocks of organosilicon resins. However, traditional organosilicon monomers, such as methyltrichlorosilane, phenyltrichlorosilane, and dimethyldichlorosilane, result in organosilicon resins with poor water solubility due to their hydrophobic Si-O-Si molecular backbone and typically nonpolar alkyl or aryl side groups. This inherent characteristic severely limits their application in water-based coatings, easy-to-clean adhesives, textile finishing agents, personal care products, and other materials requiring good water compatibility.

[0003] Researchers have attempted to improve the dispersibility of silicone resins in water by adding amphiphilic surfactants or emulsifiers to construct emulsions or microemulsions through physical blending. However, this method has significant limitations. First, the introduced surfactant may cause the resin to migrate and precipitate after curing, affecting the transparency, weather resistance, and adhesive strength of the final product. Second, this method only achieves physical dispersion and does not change the hydrophobic nature of the silicone molecules themselves. The stability of the emulsion system is often constrained by conditions such as pH, temperature, and storage time, making it prone to demulsification and stratification, and unable to achieve long-term stability. In addition, the addition of surfactants complicates the reaction system, increases purification steps and costs, and fails to fundamentally solve the essential problem of the water solubility of silicone monomers. For example, CN 110218521 A discloses a method for preparing a waterborne silicone resin conformal coating. This patent uses a phenyl silicone resin containing specific groups as a matrix, which is emulsified with various additives under high-speed dispersion after viscosity reduction to achieve water dispersion. However, this method relies on emulsifiers for dispersion, causing the emulsion system to face pH stability challenges in subsequent processes, thus limiting its practical application. CN 110684198 discloses a method for preparing an aqueous methylphenyl silicone resin, which uses (3-aminopropyl)triethoxysilane as a hydrophilic monomer to impart water dispersibility to the final product. Furthermore, CN 109705355 A uses unsaturated polyether or methyl acrylate as hydrophilic monomers, while CN114855462 A uses sulfonic acid groups as hydrophilic monomers to impart water dispersibility to the final product. However, the hydrophilicity provided by a single functional group is limited. To achieve good water dispersibility, a large amount of hydrophilic monomer must be added, which may lead to the sacrifice of other performance stability in the final coating during practical applications. Summary of the Invention

[0004] To overcome the bottlenecks of existing technologies, this invention provides a waterborne organosilicon monomer modified with trisulfonic acid groups and quaternary ammonium salts, its preparation method, and its application in waterborne resins. The resulting waterborne organosilicon monomer requires only a very small amount to impart excellent water dispersibility and storage stability to the organosilicon resin, and the resin film formation does not affect its inherent hydrophobicity, heat resistance, and mechanical properties. Furthermore, the preparation method is simple, the conditions are mild, the raw materials are readily available, and the post-processing is simple and efficient, indicating broad application prospects.

[0005] To solve the above-mentioned technical problems, the present invention adopts the following technical solution: A waterborne organosilicon monomer modified with trisulfonic acid group and quaternary ammonium salt is provided, the structure of which is shown below:

[0006] Where n = 0, 1, or 2.

[0007] A method for preparing the above-mentioned aqueous organosilicon monomer modified with trisulfonic acid group and quaternary ammonium salt is provided, and the reaction formula is shown below:

[0008]

[0009] Where n = 0, 1, or 2; The preparation method includes the following steps: 1) An amino alcohol compound reacts with 1,3-propanesulfonic acid lactone via a nucleophilic addition reaction to give intermediate 1; 2) The intermediate 1 obtained in step 1) is reacted with isocyanate triethoxysilane in the presence of a catalyst to obtain an aqueous organosilicon monomer modified with trisulfonic acid group and quaternary ammonium salt.

[0010] According to the above scheme, in step 1), the reaction temperature is 40-100 ℃ and the reaction time is 4-24 h.

[0011] According to the above scheme, in step 1), the amino alcohol compound and 1,3-propanesulfonic acid lactone are in a molar ratio of 1:2.5-3.5, preferably 1:2.8-3.2.

[0012] According to the above scheme, in step 1), after the reaction is complete, the mixture is directly filtered and dried to obtain intermediate 1.

[0013] According to the above scheme, the reaction solvents in steps 1) and 2) are independently selected from one or a combination of acetone, butanone, acetonitrile, tetrahydrofuran, N,N-dimethylformamide, and dimethyl sulfoxide.

[0014] Preferably, the mass-to-volume ratio of the amino alcohol compound to the solvent used in step 1) is 0.001–0.2 g: 1 mL, more preferably 0.05–0.1 g: 1 mL.

[0015] Preferably, the mass-to-volume ratio of intermediate 1 to the solvent used in step 2) is 0.001–0.2 g:1 mL, more preferably 0.05–0.15 g:1 mL.

[0016] According to the above scheme, in step 2), the reaction temperature is 40-80 ℃ and the reaction time is 2-8 h.

[0017] According to the above scheme, in step 2), the molar ratio of intermediate 1 and isocyanate triethoxysilane is 1-1.2:1, preferably 1-1.05:1.

[0018] According to the above scheme, in step 2), the catalyst is one or a mixture of several of the following: dibutyltin dilaurate, stannous octoate, dibutyltin diacetate, zinc octoate, and bismuth neodecanoate.

[0019] According to the above scheme, in step 2), the mass ratio of catalyst to intermediate 1 is 0.001 to 0.05:1, more preferably 0.005 to 0.01:1.

[0020] According to the above scheme, in step 2), after the reaction is completed, the solvent is evaporated under reduced pressure to obtain the target product.

[0021] This invention provides an application of the above-mentioned waterborne organosilicon monomer in the preparation of waterborne organosilicon resin.

[0022] According to the above scheme, the application is as follows: waterborne organosilicon monomers and organosilicon monomers are used as mixed monomers to prepare waterborne organosilicon resins; wherein the mass ratio of waterborne organosilicon monomers in the mixed monomers is 0.1-0.5%; preferably 0.3-0.5%.

[0023] A waterborne organosilicon resin is provided, which is prepared by hydrolysis and polycondensation reaction under acidic conditions using the above-mentioned waterborne organosilicon monomer and organosilicon monomer as mixed monomers.

[0024] According to the above scheme, the mass percentage of water-based organosilicon monomer in the mixed monomer is 0.1-0.5%; preferably 0.3-0.5%.

[0025] According to the above scheme, the reaction temperature is 50-100 ℃ and the reaction time is 1-4 h.

[0026] According to the above scheme, the organosilicon monomer is one or more of methyltrimethoxysilane, dimethyldimethoxysilane, trimethylmethoxysilane, ethyltrimethoxysilane, propyltrimethoxysilane, dipropyldimethoxysilane, and methylpropyldimethoxysilane, or a mixture thereof.

[0027] According to the above scheme, the acidic condition refers to the addition of 0.018-0.022% hydrochloric acid aqueous solution, wherein the mass-volume ratio of organosilicon monomer to hydrochloric acid is 1g:0.3-0.6 mL, preferably 1g:0.4-0.6 mL.

[0028] A method for preparing the above-mentioned waterborne organosilicon resin is provided, comprising the following steps: 1) The aqueous organosilicon monomer and the organosilicon monomer are subjected to a hydrolysis-condensation reaction under acidic conditions; 2) Then a neutralizing agent is added to the system, and the low-boiling-point hydrolysis products are removed under reduced pressure to obtain an aqueous organosilicon resin.

[0029] According to the above scheme, in step 1), the reaction temperature is 50-100 ℃ and the reaction time is 1-4 h.

[0030] According to the above scheme, in step 1), the mass percentage of the water-based organosilicon monomer in the mixed monomer is 0.1-0.5%; preferably 0.3-0.5%.

[0031] According to the above scheme, in step 1), the organosilicon monomer is one or more of methyltrimethoxysilane, dimethyldimethoxysilane, trimethylmethoxysilane, ethyltrimethoxysilane, propyltrimethoxysilane, dipropyldimethoxysilane, and methylpropyldimethoxysilane, or a mixture thereof.

[0032] According to the above scheme, in step 2), the neutralizing agent is one or a mixture of two of aminotrimethoxysilane and hexamethyldisilazane. The mass-to-volume ratio of the neutralizing agent to hydrochloric acid is 0.002-0.005 g:1 mL, preferably 0.003-0.004 g:1 mL.

[0033] According to the above scheme, in step 2), the decompression conditions are -0.05 MPa to -0.1 MPa, the temperature is 30-80 ℃, and the time is 0.1-4 h.

[0034] A water-based silicone resin coating is provided, which is prepared by fully dispersing the above-mentioned water-based silicone resin with water to obtain a coating; the obtained coating is applied to the surface of a substrate and cured by heating.

[0035] According to the above scheme, the solid content in the coating is 30-80%, preferably 40-70%.

[0036] According to the above scheme, the dispersion method is either ultrasonic dispersion or high-speed shear dispersion. Preferably, the ultrasonic time is 5–60 min; the rotation speed is 200–1500 r / min; and the time is 0.5–3 h.

[0037] According to the above scheme, the coating process is: scraping, spin coating, spraying or dipping.

[0038] According to the above scheme, the heat curing process is as follows: the temperature range is 100~220℃, and the time range is 1~3 h.

[0039] According to the above scheme, the substrate includes a non-metallic substrate and a metallic substrate; the non-metallic substrate is selected from glass plate, PE plate or silicone rubber plate, and the metallic substrate is selected from copper plate, aluminum plate or iron plate.

[0040] According to the above scheme, the substrate undergoes pretreatment, which includes the following steps: first ultrasonic treatment of the substrate with acetone, second ultrasonic treatment of the first ultrasonic-treated substrate with deionized water, and then drying. The conditions for the first ultrasonic treatment are: room temperature and time of 5–25 min. The conditions for the second ultrasonic treatment are: room temperature and time of 5–25 min. The drying process is performed by blowing with high-purity nitrogen or drying in an oven.

[0041] According to the above scheme, the coating thickness is 1 to 500 μm.

[0042] According to the above scheme, the static angle range of the coating is 95°-105°.

[0043] According to the above scheme, the friction distance of the coating is 21-23 m.

[0044] According to the above scheme, the adhesion level of the coating ranges from 4B to 5B.

[0045] Compared with the prior art, the technical solution of the present invention has the following beneficial effects: 1. This invention provides a waterborne organosilicon monomer modified with trisulfonic acid groups and quaternary ammonium salts. By simultaneously introducing three sulfonic acid groups and one quaternary ammonium salt group, a synergistic effect is generated, significantly enhancing molecular polarity and hydration capacity, thereby endowing the monomer with excellent water solubility. When the obtained waterborne organosilicon monomer is used to prepare waterborne organosilicon resins, a self-emulsifying effect can be formed without relying on surfactants. Only a very small amount needs to be added to effectively reduce the interfacial energy of the system. The resulting waterborne organosilicon resin achieves excellent dispersion stability.

[0046] 2. When the waterborne organosilicon monomer of the present invention is used to prepare waterborne organosilicon resin, it can form a stable water dispersion system while effectively avoiding the damage to the resin's intrinsic properties caused by common additives. At the same time, at low addition levels, it does not sacrifice the inherent core properties of organosilicon resin, such as heat resistance, mechanical strength, and stability, thus overcoming the performance trade-off problem in traditional waterborne modification and ensuring the reliability of the material in harsh environments.

[0047] 3. The present invention also provides a method for preparing the above-mentioned water-based organosilicon monomer. The preparation method is simple and efficient, with a simplified synthetic route and mild reaction conditions. It achieves simple and efficient separation and purification through its own water solubility, without the need for complex post-processing. The overall process has high yield, easy control of impurities, is green and environmentally friendly, and has controllable costs. It has good potential for large-scale production and can meet the industrialization needs of high-performance water-based additives. Attached Figure Description

[0048] To more clearly illustrate the technical solutions of the embodiments of the present invention, the accompanying drawings of the embodiments will be briefly described below.

[0049] Figure 1 In Example 2, the waterborne silicone resin was prepared as a coating with a solid content of 50% using water as a solvent, and the viscosity change was observed after 0-30 days of storage.

[0050] Figure 2 Comparison of the hydrophobic angles of the aqueous resin (left) prepared by the modified organosilicon monomer in Example 3 and the commercially available methyl silicone resin (right) after coating.

[0051] Figure 3 Comparison of adhesion properties of waterborne resin (left) prepared by modified organosilicon monomer in Example 3 and commercially available methyl silicone resin (right) after coating.

[0052] Figure 4 Comparison of hardness of waterborne resin (left) prepared by modified organosilicon monomer in Example 3 and commercially available methyl silicone resin (right) after coating. Detailed Implementation

[0053] The following detailed description of specific embodiments of the present invention is part of this specification. The principles of the present invention are illustrated through examples, and other aspects, features and advantages of the present invention will become apparent from this detailed description.

[0054] The substrate in the following embodiment is a tinplate. The tinplate is pretreated in the following ways: the tinplate is subjected to a first ultrasonic treatment with acetone for 10 minutes; then it is subjected to a second ultrasonic treatment with deionized water for 10 minutes; finally, it is placed in an 80°C drying oven for 15 minutes.

[0055] Unless otherwise specified, all raw materials used in this invention are commercially available.

[0056] Example 1: The molecular structure and synthetic route of the organosilicon monomer modified by trisulfonic acid group and quaternary ammonium salt when n=1 are shown below:

[0057] (1) Synthesis of intermediate 1 3-Aminopropanol (10 g, 0.133 mol) and 1,3-propanesulfonic acid lactone (48.73 g, 0.399 mol) were added to 200 mL of acetone and stirred at 50 °C for 20 h. After cooling to room temperature, a large amount of solid precipitated out. After vacuum filtration and drying, 157.6 g of intermediate was obtained, with a yield of 97.8%.

[0058] (2) Synthesis of modified organosilicon monomers Intermediate 1 (10 g, 22.6 mmol), isocyanate triethoxysilane (5.59 g, 22.6 mmol), and catalyst dibutyltin dilaurate (50 mg) were added to 200 mL of tetrahydrofuran and reacted at 60 °C for 4 h. The solvent was then removed under reduced pressure to obtain 15.3 g of the target product, yield: 98.1%.

[0059] Example 2: Preparation of waterborne organosilicon resin The aqueous organosilicon monomer (0.5 g) modified with trisulfonic acid group and quaternary ammonium salt obtained in Example 1 and methyltrimethoxysilane (124 g) were added to a round-bottom flask, wherein the aqueous organosilicon monomer accounted for 0.4% by mass. The two were mixed evenly, and then hydrochloric acid (0.02%, 50 mL) was added. The mixture was heated to 60°C and stirred for 2 h. Finally, 0.175 g of hexamethyldisilazane was added. The pressure was set to -0.09 MPa and the temperature to 60°C. The solvent was removed by distillation for 1 h, yielding 121.5 g of aqueous organosilicon resin, with a yield of 98.6%.

[0060] Example 3: Performance Testing of Waterborne Organosilicon Resin The aqueous silicone resin obtained in Example 2 was prepared into an aqueous solution with a solid content of 50%, and stirred at 500 r for 30 min to obtain a coating. The coating was then sprayed onto an iron plate test piece to form a film, and cured at 120°C for 2 h to obtain the coating.

[0061] Comparative Example 1 Commercially available methyl silicone resin was prepared into a 50% solids solution using butyl acetate as a solvent. The solution was stirred at 500 rpm for 30 min and then sprayed onto an iron plate test piece to form a film. The film was cured at 120°C for 2 h to obtain the coating, which is Comparative Example 1.

[0062] In Example 3 and Comparative Example 1, the film thickness was approximately 60 μm. The hydrophobicity, hardness, abrasion resistance, adhesion, and heat resistance of the two coatings were tested, as shown in Table 1. The testing methods for stability, hydrophobicity, adhesion, and abrasion resistance were as follows: The method for testing the dispersibility and stability of the water-based resin is as follows: Approximately 500 mL of the coating sample is placed in a sealed tin can with a lid, and then placed in a constant temperature oven at 30±2℃ for 0 to 30 days. During this period, the sample is removed every 5 days to observe for flocculation, agglomeration, demulsification, or a significant increase in viscosity, and viscosity is measured simultaneously. No flocculation, agglomeration, demulsification, or viscosity change is considered "good" dispersibility; the presence of flocculation, agglomeration, demulsification, or viscosity change is considered "poor" dispersibility. The viscosity change data for Example 3 are as follows: Figure 1 As shown.

[0063] The hydrophobicity test was performed using a contact angle meter (OCA20). At room temperature, 5 μL of distilled water was dropped onto the coating surfaces prepared in Example 3 and Comparative Example 1, and the contact angles were measured. The results are shown in Table 1. Figure 2 As shown.

[0064] The wear resistance test is conducted according to the reciprocating motion wear test method to detect the wear resistance of the superhydrophobic coating: 1000-grit sandpaper is fixed on the table as the wear surface, so that the coating is in direct contact with the sandpaper, and a 100 g weight is placed on the sample as the wear load.

[0065] The adhesion test was conducted according to the ASTM D3359 cross-cut adhesion test to determine the adhesion of the superhydrophobic coating. The coating was cut into a grid using a cross-cutting tool; surface impurities were lightly brushed away; the tape was placed parallel to the grid lines in the middle and smoothed by hand; the tape was then torn at approximately a 60° angle, and the cut area was examined. The coating's adhesion was defined as 0B-5B grade based on the area of ​​peeling, with 0B indicating extremely poor adhesion and 5B indicating excellent adhesion. Table 1 shows that the superhydrophobic coating prepared in this embodiment achieved an adhesion grade of 4B-5B. Figure 3 As shown.

[0066] The coating hardness was tested using the pencil hardness method: A set of calibrated drawing pencils from 6B to 9H were prepared, with the leads sharpened to 5–6 mm and the ends smoothed. The sample was placed on a hard, horizontal surface. During testing, the pencil was held at a 45° angle to the sample, and a load of 750 g was applied. Starting with a harder pencil (e.g., 3H), the pencil was used to draw approximately 2 cm on the coating surface at a uniform speed. After removing debris with a soft cloth, the scratch was observed at a 45° angle under sufficient light. Permanent grooves that could not be erased were considered "scratches," while erasable graphite marks without coating damage were considered "no scratches." The test was iterated, using a softer pencil for scratches and a harder pencil for no scratches. The hardest pencil grade, where no scratches were observed in both tests, was taken as the coating hardness value. The test results are as follows: Figure 4 As shown.

[0067] Table 1. Performance comparison of Example 3 and Comparative Example 1

[0068] Table 1 shows that, thanks to the unique molecular design of the obtained waterborne organosilicon monomer, the silicone resin prepared based on it exhibits significant comprehensive advantages. It not only possesses excellent water solubility, enabling rapid dispersion in water and the formation of a highly stable aqueous dispersion system, greatly facilitating subsequent processing and applications; more importantly, while achieving excellent hydrophilic properties, its key end-use performance is not compromised. Rigorous testing revealed that the resin's performance in core performance indicators such as hydrophobicity, abrasion resistance, adhesion to substrates, and high-temperature stability is comparable to commercially available samples, with no significant differences. This fully demonstrates that the waterborne organosilicon monomer successfully overcomes the performance trade-offs often faced by traditional waterborne products. In addition to endowing the material with green, environmentally friendly, and easy-to-handle waterborne characteristics, it fully retains the inherent high-performance characteristics of organosilicon materials, achieving a perfect unity of environmental friendliness and excellent comprehensive performance.

[0069] Examples 4-9: Referring to the preparation methods of Examples 1-3, the types of raw materials (i.e., n values) of amino alcohol compounds were changed, and the process parameters in the reaction, such as the raw material molar ratio, solvent, reaction temperature, reaction time, catalyst, etc., were changed. A series of experiments were conducted to obtain different modified monomers. Subsequently, waterborne resins were prepared using the obtained modified organosilicon monomers (specific steps are the same as in Example 2). The core parameters of dispersibility and hydrophobic angle after the resin film was coated (specific coating method is the same as in Example 3) were tested. Experiments of Examples 4-9 were organized, and the specific results are shown in Table 2.

[0070] Table 2. Specific parameters and test performance of Examples 4-9

[0071] The results in the table show that by adjusting the types of raw materials (i.e., the n-value) and systematically changing the key process parameters (including molar ratio, solvent, reaction temperature, reaction time, and catalyst), a series of modified monomers with different structures were synthesized. Aqueous resins prepared based on the obtained modified monomers all exhibited good water dispersibility. Furthermore, coatings prepared from these resins maintained a stable hydrophobic angle between 95° and 100°.

[0072] The above description is merely a preferred embodiment of the present invention, and should not be construed as limiting the scope of the invention. It should be noted that those skilled in the art can make various improvements and modifications without departing from the principles of the present invention, and these improvements and modifications are also considered to be within the scope of protection of the present invention.

Claims

1. A waterborne organosilicon monomer based on trisulfonic acid group and quaternary ammonium salt modification, characterized in that, The structure of the aqueous organosilicon monomer is as follows: Wherein, n=0, 1, or 2.

2. A method for producing the aqueous organosilicon monomer based on a trisulfonic acid group and a quaternary ammonium salt modification according to claim 1, characterized by, The reaction formula is as follows: Wherein, n=0, 1, or 2; The preparation method comprises the following steps: 1) nucleophilic addition reaction of amino alcohol compound and 1, 3-propane sultone to obtain intermediate 1; 2) addition reaction of intermediate 1 obtained in step 1) and isocyanate triethoxysilane under the action of a catalyst, to obtain the aqueous organosilicon monomer modified based on trisulfonic acid group and quaternary ammonium salt.

3. The method of claim 2, wherein, In step 1), the reaction temperature is 40-100℃, and the reaction time is 4-24 h; in step 2), the reaction temperature is 40-80℃, and the reaction time is 2-8 h.

4. The preparation method of claim 2, wherein, In step 1), the molar ratio of amino alcohol compound to 1, 3-propane sultone is 1:2.5-3.5; In step 2), the molar ratio of intermediate 1 to isocyanate triethoxysilane is 1-1.2:1; the mass ratio of catalyst to intermediate 1 is 0.001-0.05:1; and the catalyst is one or a mixture of several of dibutyltin dilaurate, stannous octoate, dibutyltin diacetate, zinc octoate, and bismuth neodecanoate.

5. Application of the aqueous organosilicon monomer of claim 1 in the preparation of an aqueous organosilicon resin.

6. An aqueous silicone resin characterized by, The aqueous organosilicon monomer of claim 1 and an organosilicon monomer are used as mixed monomers to prepare the aqueous organosilicon resin by hydrolytic polycondensation reaction under acidic conditions.

7. The aqueous organosilicon resin of claim 6, wherein, The mass proportion of the aqueous organosilicon monomer in the mixed monomers is 0.1-0.5%; The reaction temperature is 50-100℃, and the reaction time is 1-4 h; The organosilicon monomer is a mixture of one or more of methyltrimethoxysilane, dimethyldimethoxysilane, trimethylmethoxysilane, ethyltrimethoxysilane, propyltrimethoxysilane, dipropyl dimethoxysilane, and methylpropyl dimethoxysilane.

8. The aqueous silicone resin according to claim 6, characterized in that, The acidic conditions refer to the addition of 0.018-0.022% hydrochloric acid aqueous solution, wherein the mass-volume ratio of organosilicon monomer to hydrochloric acid is 1g:0.3-0.6 mL.

9. An aqueous silicone resin coating, characterized by, The aqueous organosilicon resin of claim 6 is coated on the surface of a substrate to prepare the same.

10. A method of preparing the aqueous silicone resin coating of claim 9, characterized in that, The aqueous organosilicon resin of claim 6 is dispersed in water to prepare a coating material, which is coated on the surface of a substrate and cured by heating to prepare the same; wherein the heating and curing process is as follows: the temperature range is 100-220℃, and the time range is 1-3 h.

Citation Information

Patent Citations

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    CN109705355A

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