Cationic microemulsion water-displacing quick-drying agent, preparation method and application thereof

Abstract

The application belongs to the technical field of fine chemical industry, and particularly relates to a cationic microemulsion water-repellent quick-drying agent and a preparation method and application thereof. The cationic microemulsion water-repellent quick-drying agent is prepared by using Arquad 2C-75 (dicoconut alkyl dimethyl ammonium chloride) as a core cationic component, compounding refined white oil, matching a surfactant, a coupling agent and deionized water to construct a microemulsion system, mixing an oil phase, preparing a water phase, primary emulsifying, high-pressure homogenizing and post-treating. The product prepared by the application has a contact angle greater than 110 degrees, a sliding time shortened by more than 31.4%, is stable without precipitation in the range of-10 DEG C to 50 DEG C, has a viscosity less than 100 cP and can be dissolved and used immediately, is compatible with an anion system, has no ethanol / toluene solvent, VOCs detection meets the limit value of GB38508-2020, and has excellent performance in water-repellent quick-drying on the surface of an automobile and a wide application range.

Description

Technical Field

[0001] This invention belongs to the field of fine chemical technology, specifically relating to a cationic microemulsion water-repellent quick-drying agent, its preparation method, and its application. Background Technology

[0002] Automotive surface water-repellent and quick-drying agents are an important category of fine chemicals in automotive care. They primarily work by forming a hydrophobic film on automotive paint and glass surfaces, enabling water droplets to slide off quickly, surfaces to dry rapidly, reducing water residue, and enhancing paint gloss. Currently, traditional products on the market generally use chemical systems with amino silicone oils (such as polyquaternium 6922) as the core component. This system has advantages such as strong hydrophobic film-forming properties, significant gloss enhancement effects, and simple preparation processes, thus enjoying widespread application. However, with increasing environmental awareness, this system is gradually showing many technical bottlenecks in meeting the requirements of green chemistry and convenient application, making it difficult to adapt to the new demands of industry development. The main drawbacks are as follows: First, the synthesis process of amino silicone oil-based water-repellent and quick-drying agents is highly dependent on organic solvents such as toluene and n-hexane, resulting in significant VOC emissions during production and application, causing a significant impact on the environment. Second, at low temperatures (<5℃), this system is prone to precipitation and stratification, losing its performance. Simultaneously, its high viscosity (>500 cP) and slow dissolution rate require specialized stirring or dilution equipment, making on-site dissolution and use impossible. Furthermore, the rigidity of amino silicone oil molecules makes it difficult to form a continuous, dense hydrophobic film on automotive surfaces, resulting in a water contact angle generally below 100°, slow water droplet sliding, and long drying time. Coupled with high raw material costs and large unit dosages, the overall economic efficiency is poor. These defects, to some extent, limit the application of water-repellent and quick-drying agents.

[0003] Therefore, it is crucial to develop a new type of water-repellent and quick-drying agent that is compatible, environmentally friendly and low-emission, stable over a wide temperature range, easy to apply, and highly efficient in water removal. Summary of the Invention

[0004] To address the aforementioned challenges, this invention provides a cationic microemulsion water-repellent and quick-drying agent. By optimizing the synergistic effect of cationic surfactants and low-viscosity isoalkanes, it achieves efficient water repellency, rapid drying, and wide-temperature stability, while also being environmentally friendly and economical.

[0005] To achieve the above objectives, the technical solution adopted by the present invention is as follows: A cationic microemulsion water-repellent and quick-drying agent comprises the following components and their mass percentages: 10-20% biscocarbamoyl dimethyl ammonium chloride (Arquad 2C-75), 5-10% surfactant, 1-5% coupling agent, 25-35% refined white oil, and the balance being deionized water.

[0006] This invention uses di-cocoyl dimethyl ammonium chloride instead of amino silicone oil as the cationic water-repellent core. Its dialkyl chains can be oriented onto the substrate surface, significantly reducing surface tension and promoting rapid water droplet sliding. It also possesses pseudo-wax properties, forming a high-gloss film without water spot residue. This component is bio-based, sulfur-free, and aromatic-free, making it environmentally friendly and compatible with both anionic and nonionic systems. It solves the problems of silica spots and low-temperature precipitation in traditional systems. Refined white oil, as the oil phase core, is a low-viscosity isoalkanes with a pour point as low as -20°C, providing highly efficient hydrophobic groups. It synergistically works with the cationic component to achieve stability across the entire temperature range of -10°C to 50°C (conventional products precipitate at -5°C); simultaneously, it fills in molecular gaps, accelerating water droplet aggregation and sliding. This invention utilizes the low surface tension (28 mN / m) of refined white oil and the directional arrangement of cationic surfactants to form a microemulsion structure, constructing a superhydrophobic film (contact angle > 110°); the ultra-low viscosity (< 100 cP, the product viscosity can be directly measured using a digital viscometer) formula enables instant dissolution and use, breaking through the equipment dependence of traditional high viscosity systems.

[0007] Meanwhile, this invention uses deionized water as the dispersion medium, with a mineralization of ≤50mg / L, which avoids reactions between ions and cationic components in the water, ensuring the stability of the product system, reducing product costs, and enabling immediate use after aqueous dilution. The system of this invention is compatible with anionic and nonionic systems, completely avoiding the risk of silica spots.

[0008] Preferably, the cationic microemulsion water-repellent and quick-drying agent comprises the following components and their mass percentages: 13-18% biscocarbamate dimethylammonium chloride, 6-8% surfactant, 2-4% coupling agent, 28-32% refined white oil, and the balance being deionized water.

[0009] Preferably, the cationic microemulsion water-repellent and quick-drying agent is composed of the following components and their mass percentages: 15% biscocarbamate dimethylammonium chloride, 7% surfactant, 3% coupling agent, 30% refined white oil, and the balance being deionized water.

[0010] Preferably, the surfactant is isomeric deca-ol polyoxyethylene ether (XL-90, EO=7); the coupling agent is ethylene glycol butyl ether.

[0011] This invention further selects isomeric decaethylene glycol polyoxyethylene ether with EO=7 as a surfactant, which can effectively control the HLB value of the microemulsion between 8 and 10, enhance the low-temperature stability of the product, and improve the emulsification effect of the oil-water phase, ensuring the uniformity of the microemulsion system; ethylene glycol butyl ether is used as a coupling agent to improve the compatibility between the oil phase and the water phase, promote the uniform dispersion of each component, accelerate solvent evaporation, and improve the quick-drying performance of the product.

[0012] Preferably, the refined white oil is an isoparaffin with a flash point of 135~140℃ and a purity of ≥99.5%; the deionized water has a mineralization of ≤50mg / L.

[0013] The refined white oil of this invention preferably uses G3H white oil, which is an isoparaffin with a flash point of 135-140℃ and a purity of ≥99.5%. Its low surface tension (28 mN / m) and the directional alignment of the cationic surfactant form a superhydrophobic film (contact angle >110°), providing hydrophobic groups and rapid drying properties for the microemulsion. The final product obtained by this invention has a particle size of 100-200 nm, inhibits Ostwald ripening, and achieves stability across the entire temperature range from -10℃ to 50℃. The deionized water salinity is controlled within the range of ≤50 mg / L to avoid instability of the cationic components. These effects stem from the directional alignment of the dialkyl chains of the bis-cocoyl dimethyl ammonium chloride, synergistically forming a dense hydrophobic film with the help of the low-pour-point isoparaffin white oil, thereby achieving a high contact angle and rapid sliding.

[0014] The present invention also provides a method for preparing the aforementioned cationic microemulsion water-repellent and quick-drying agent, comprising the following steps: S1. Oil phase mixing: Heat the refined white oil to 38~45℃, then add the coupling agent and stir until transparent to obtain solution I; S2, Aqueous phase preparation: Add biscocarbamate dimethylammonium chloride and surfactant to deionized water, stir in a water bath until homogeneous, and obtain solution II; S3. Pre-emulsification: Solution II obtained in step S2 is added dropwise to solution I obtained in step S1 at a rate of 1~3 mL / min, and a high-speed shear machine is turned on simultaneously to emulsify and form a pre-emulsion. S4. High-pressure homogenization: The pre-emulsion obtained in step S3 is transferred to a high-pressure homogenizer for homogenization to obtain a semi-transparent microemulsion. S5. Post-processing: The semi-transparent microemulsion obtained in step S4 is filtered through a sieve at 24~28℃ to remove small amounts of impurities and large particles from the system, thus obtaining the final product.

[0015] Preferably, the stirring conditions in step S1 to achieve transparency are stirring at a speed of 200-400 rpm for 10-15 minutes; the stirring conditions in step S2 to achieve uniform mixing in a water bath are stirring in a water bath at 40-50°C for 10-20 minutes.

[0016] Preferably, during emulsification in step S3, the rotation speed is 7000~9000 rpm and the emulsification time is 10~15 min; the homogenization conditions in step S4 are to cycle homogenize 3~5 times under a pressure of 45~55 MPa and control the particle size to be 100-200 nm.

[0017] This invention heats the refined white oil to 38-45°C to reduce the viscosity of G3H white oil, promoting uniform mixing with the coupling agent (ethylene glycol butyl ether) and preventing localized agglomeration. Controlling the water bath temperature at 40-50°C increases the dissolution rate of the cationic surfactant, ensuring the homogeneity and transparency of the aqueous phase system. Adding the aqueous phase at a low rate of 1-3 mL / min avoids oil-water separation, while high-speed shearing achieves preliminary microemulsification, laying the foundation for subsequent high-pressure homogenization. High-pressure homogenization refines the emulsion particles to the nanoscale, significantly improving the stability of the microemulsion.

[0018] The present invention also provides the application of the aforementioned cationic microemulsion water-repellent and quick-drying agent in the preparation of car wash products.

[0019] The present invention also provides a car wash product, characterized in that it includes the aforementioned cationic microemulsion water-repellent and quick-drying agent, the mass percentage of which is 0.1~0.3%.

[0020] The car wash products described in this invention include car wash liquid, cleaning agents, etc.

[0021] Dicarboxylic dimethyl ammonium chloride, as a bio-based cationic surfactant, possesses strong interfacial activity, pseudo-wax properties, and excellent compatibility. Refined white oil, a low-viscosity isoalkanes, has an extremely low pour point and provides highly efficient hydrophobic groups. This invention combines the two to construct a microemulsion system, achieving a significant performance leap in the water-repellent and quick-drying agent. This effectively expands the effective range of the quick-drying agent.

[0022] Therefore, compared with the prior art, the present invention has the following advantages: (1) The present invention uses dicoalkyl dimethyl ammonium chloride as the core component. Its dialkyl chains are oriented to form a low-energy surface, so that the water contact angle of the product at a concentration of 0.3% reaches 112.5°±1.2°. Compared with traditional amino silicone oil products, it has higher water removal efficiency while effectively reducing the concentration used.

[0023] (2) Products made using the cationic microemulsion water-repellent quick-drying agent of the present invention do not precipitate or separate into layers in the full temperature range of -10℃ to 50℃. They remain transparent and uniform even after being placed at -10℃ for 7 days. This solves the problem of crystallization and precipitation of traditional amino silicone oil products at <5℃ and expands the application temperature range of the products. (3) The product of this invention uses bio-based coconut oil as the core component, with biodegradable components accounting for >80%, and contains no organic solvents such as toluene and n-hexane. VOCs emissions are reduced, which meets the requirements of EU REACH Regulation (EC 1907 / 2006) and national GB38508-2020 VOCs emission limits. (4) The preparation method of the present invention includes only five steps: oil phase mixing, aqueous phase preparation, primary emulsification, high pressure homogenization and post-treatment. The process parameters of each step are clear, the equipment is conventional equipment in the fine chemical industry, no special customized equipment is required, the process has good repeatability, the product batch consistency is high, and it is suitable for large-scale industrial production. Detailed Implementation

[0024] The present invention will be further described below with reference to embodiments. These embodiments are provided to facilitate understanding of the invention and are not intended to limit the invention. Those skilled in the art can make various modifications based on the basic idea of ​​the invention, but all modifications are within the scope of the invention as long as they do not depart from its fundamental spirit.

[0025] The dicoalkyl dimethyl ammonium chloride can be purchased from Jining Tangyi Chemical Co., Ltd.; the refined white oil G3H can be purchased from Total, France, CAS No. 64742-46-7; the isomeric deca-ol polyoxyethylene ether can be purchased from Zhejiang Deyuan Chemical Co., Ltd., CAS No. 61827-42-7; the ethylene glycol butyl ether can be purchased from Ningbo Sapphire Petrochemical Co., Ltd., CAS No. 111-76-2.

[0026] The traditional quick-drying agent formula used in this experiment consists of the following components and their mass percentages: 30% amino silicone oil (molecular weight 5000-8000, available from Shandong Dayi Chemical Co., Ltd.); 10% isomeric tridecyl alcohol polyoxyethylene ether (purchased from Shenzhen Jihechang New Materials Co., Ltd., product name 1308, CAS number 9043-30-5, HLB 13); 5% ethanol; and 55% deionized water.

[0027] Example 1: A cationic microemulsion water-repellent and quick-drying agent The cationic microemulsion water-repellent and quick-drying agent is composed of the following components and their mass percentages: 10% biscocarbamoyl dimethyl ammonium chloride (Arquad 2C-75), 5% EO=7 isomeric decayl alcohol polyoxyethylene ether, 1% ethylene glycol butyl ether, 25% refined G3H white oil, and the balance being deionized water.

[0028] The preparation method of the aforementioned cationic microemulsion water-repellent and quick-drying agent includes the following steps: S1. Oil phase mixing: Heat the refined G3H white oil to 38°C, then add ethylene glycol butyl ether and stir at 200 rpm for 15 minutes until transparent to obtain solution I; S2, Aqueous phase preparation: Add biscocarbamate dimethylammonium chloride and EO=7 isomeric decayl alcohol polyoxyethylene ether to deionized water, then heat to 40°C in a water bath and stir for 20 min until the mixture is homogeneous to obtain solution II; S3. Pre-emulsification: Solution II obtained in step S2 is added dropwise to solution I obtained in step S1 at a rate of 1 mL / min, and a high-speed shear machine is simultaneously turned on at room temperature and 7000 rpm for 15 min to emulsify, forming a pre-emulsion. S4. High-pressure homogenization: The pre-emulsion obtained in step S3 is transferred to a high-pressure homogenizer and homogenized three times at room temperature and 45 MPa to control the particle size to about 100 nm, thereby obtaining a semi-transparent microemulsion. S5. Post-processing: The semi-transparent microemulsion obtained in step S4 is filtered through a 200-mesh sieve at 24°C to obtain the final product.

[0029] Example 2: A cationic microemulsion water-repellent and quick-drying agent The cationic microemulsion water-repellent and quick-drying agent is composed of the following components and their mass percentages: 20% biscocarbamate dimethylammonium chloride, 10% EO=7 isomeric decayl alcohol polyoxyethylene ether, 5% ethylene glycol butyl ether, 35% refined G3H white oil, and the balance being deionized water.

[0030] The preparation method of the aforementioned cationic microemulsion water-repellent and quick-drying agent includes the following steps: S1. Oil phase mixing: Heat the refined white oil to 45°C, then add ethylene glycol butyl ether and stir at 400 rpm for 10 minutes until transparent to obtain solution I; S2, Aqueous phase preparation: Add biscocarbamate dimethylammonium chloride and EO=7 isomeric decayl alcohol polyoxyethylene ether to deionized water, heat in a water bath to 50°C, stir and dissolve for 10 min until uniformly mixed to obtain solution II; S3. Pre-emulsification: Solution II obtained in step S2 is added dropwise to solution I obtained in step S1 at a rate of 3 mL / min, and a high-speed shear machine is turned on simultaneously to emulsify at 9000 rpm at room temperature for 10 min to form a pre-emulsion. S4. High-pressure homogenization: The pre-emulsion obtained in step S3 is transferred into a high-pressure homogenizer and homogenized three times at room temperature and 55 MPa to control the particle size to 200 nm, thereby obtaining a semi-transparent microemulsion. S5. Post-processing: The semi-transparent microemulsion obtained in step S4 is filtered through a 200-mesh sieve at 28°C to obtain the final product.

[0031] Example 3: A cationic microemulsion water-repellent and quick-drying agent The cationic microemulsion water-repellent and quick-drying agent comprises the following components and their mass percentages: 18% biscocarbamate dimethylammonium chloride, 6% EO=7 isomeric decayl alcohol polyoxyethylene ether, 5% ethylene glycol butyl ether, 25% refined G3H white oil, and the balance being deionized water.

[0032] The preparation method of the aforementioned cationic microemulsion water-repellent and quick-drying agent includes the following steps: S1. Oil phase mixing: Heat the refined white oil to 42°C, then add ethylene glycol butyl ether and stir at 300 rpm for 10 minutes until transparent to obtain solution I; S2, Aqueous phase preparation: Add biscoalkyldimethylammonium chloride and EO=7 isomeric decayl alcohol polyoxyethylene ether to deionized water, heat to 45°C in a water bath, stir for 15 min until uniformly mixed, and obtain solution II; S3. Pre-emulsification: Solution II obtained in step S2 is added dropwise to solution I obtained in step S1 at a rate of 2 mL / min, and a high-speed shear machine is turned on simultaneously. The mixture is emulsified at room temperature and 8000 rpm for 10 min to form a pre-emulsion. S4. High-pressure homogenization: The pre-emulsion obtained in step S3 is transferred into a high-pressure homogenizer and homogenized three times at room temperature and pressure of 50 MPa to obtain a semi-transparent microemulsion. S5. Post-processing: The semi-transparent microemulsion obtained in step S4 is filtered through a 200-mesh sieve at 25°C to obtain the final product.

[0033] Example 4: A cationic microemulsion water-repellent and quick-drying agent The cationic microemulsion water-repellent and quick-drying agent comprises the following components and their mass percentages: 18% biscocarbamate dimethylammonium chloride, 8% EO=7 isomeric decayl alcohol polyoxyethylene ether, 3% ethylene glycol butyl ether, 25% refined G3H white oil, and the balance being deionized water.

[0034] The preparation method of the cationic microemulsion water-repellent quick-drying agent is the same as that in Example 3.

[0035] Example 5: A cationic microemulsion water-repellent and quick-drying agent The cationic microemulsion water-repellent and quick-drying agent comprises the following components and their mass percentages: 16% biscocarbamate dimethylammonium chloride, 6% EO=7 isomeric decayl alcohol polyoxyethylene ether, 5% ethylene glycol butyl ether, 28% refined G3H white oil, and the balance being deionized water.

[0036] The preparation method of the cationic microemulsion water-repellent quick-drying agent is the same as that in Example 3.

[0037] Comparative Example 1: A water-repellent and quick-drying agent The composition and preparation method of the water-repellent and quick-drying agent are similar to those in Example 3; The difference from Example 3 is that Comparative Example 1 uses nonylphenol polyoxyethylene ether (purchased from Yuanye Biotechnology, B65867-250mg, TX-10, EO=10) instead of isomeric deca-ol polyoxyethylene ether (XL-90) with EO=7.

[0038] Comparative Example 2: A water-repellent and quick-drying agent The composition and preparation method of the water-repellent and quick-drying agent are similar to those in Example 3; The difference from Example 3 is that in Comparative Example 2, the dicoalkyldimethylammonium chloride was replaced with polyquaternium-2 (purchased from Hubei Yalong New Materials Co., Ltd., CAS No. 68555-36-2).

[0039] Comparative Example 3: A water-repellent and quick-drying agent The composition and preparation method of the water-repellent and quick-drying agent are similar to those in Example 3; The difference from Example 3 is that the concentration of Arquad 2C-75 in Comparative Example 3 was reduced to 8%.

[0040] Comparative Example 4: A water-repellent and quick-drying agent The composition and preparation method of the water-repellent and quick-drying agent are similar to those in Example 3; The difference from Example 3 is that the concentration of Arquad 2C-75 in Comparative Example 4 was increased to 25%.

[0041] Comparative Example 5: A water-repellent and quick-drying agent The composition and preparation method of the water-repellent and quick-drying agent are similar to those in Example 3; The difference from Example 3 is that in Comparative Example 5, the isomeric deca-ol polyoxyethylene ether (XL-90) with EO=7 was removed and replaced with deionized water.

[0042] Experimental Example 1 Dosage Screening 1. Test samples: cationic microemulsion water-repellent and quick-drying agent prepared in Example 3, and traditional amino silicone oil water-repellent agent; 2. Test method: The cationic microemulsion water-repellent and quick-drying agent of the present invention was diluted with concentrations of 0.1% (car wash liquid 1), 0.2% (car wash liquid 2), 0.3% (car wash liquid 3), 0.4% (car wash liquid 4), and 0.5% (car wash liquid 5) to prepare car wash liquids. At the same time, the traditional amino silicone oil water-repellent agent was prepared with concentrations of 0.3% (car wash liquid 6), 0.5% (car wash liquid 7), and 0.7% (car wash liquid 8) according to the same method to prepare car wash liquids.

[0043] The formula for other components in the car wash liquid is as follows: AEO-9 (fatty alcohol polyoxyethylene ether) 3%, sodium dodecylbenzene sulfonate 6%, EDTA-2NA 0.2%, sodium benzoate 0.1%, triethanolamine (to adjust the pH to 7), sodium chloride (for thickening) 1.5%, and deionized water to make up to 100%.

[0044] Then, the contact angles of the above eight car wash liquids were measured according to the international standard ISO 19403-2:2017 "Paints and varnishes—Wettability—Part 2: Determination of the surface free energy of solid surfaces by measuring the contact angle" at 25°C and 55% RH on a metallic car panel. 6 μL droplets of each car wash liquid were then dropped at a 15° tilt angle, with a sliding length of 100 mm and a sliding height of 25.9 mm. The sliding time and contact angle were recorded. The contact angles in Table 1 are static contact angles, measured on a horizontal panel after the droplet stabilized and before the tilt began. The droplets were directly measured using a contact angle measuring instrument. The sliding time was then calculated using the Furmidge equation. Slip time = γ(cosθR-cosθA) / pg (γ: surface tension, θR / θA: backward / forward angle) In the above equation, γ is directly measured using the WXZL308 fully automatic tension measuring instrument from Wuhan Wugao Xigao Electric Co., Ltd.; p is density, which is directly measured using a density meter; g is the acceleration due to gravity, which is taken as 10. θR and θA are dynamic contact angles, measured during the movement of the three-phase contact lines. ISO 19403-2:2017 specifies the following method: θA (advance angle): The maximum contact angle at which the three-phase lines move outward as the droplet expands.

[0045] θR (backward angle): The minimum contact angle at which the three-phase lines move inward when the droplet contracts.

[0046] This experiment used a drop test with an inclination angle of 15°. Due to the low γ value and the small difference between θR and θA, the product significantly improved the drop efficiency.

[0047] 3. Experimental results: The specific experimental results are shown in Table 1.

[0048] Table 1. Statistics on contact angle and slippage time of products at different dilution concentrations.

[0049] When the cationic microemulsion water-repellent and quick-drying agent prepared in Example 3 of this invention was used to prepare car wash liquid, it was measured that the initial sliding angle of the water droplets was only 8.2° (compared to 14.5° for traditional products), resulting in a straight and continuous slide without watermarks. Its water-repellent effect gradually increased with increasing concentration within the range of 0.1% to 0.3%, reaching its peak performance at 0.3% concentration. After this concentration, the contact angle decreased, and the sliding time increased accordingly. Compared with traditional amino silicone oil water-repellent agents (amino silicone oil molecules are highly rigid, unable to form a dense hydrophobic film, resulting in discontinuous water droplet sliding trajectories and easy residue formation), the present invention, at a concentration of only 0.1%, is superior to the traditional product at 0.5% concentration, significantly reducing the effective amount of water-repellent agent required. The contact angle of the product of this invention is 14% higher than that of traditional products, due to the low-energy surface formed by the directional arrangement of Arquad 2C-75 dialkyl chains (surface tension 28mN / m, compared to >35mN / m for traditional products), and the sliding time is shortened by 31.4% compared to traditional products.

[0050] Experiment Example 2 Stability Test 1. Test samples: Water-repellent and quick-drying agents prepared in Examples 1-5 and Comparative Examples 1-5, and traditional amino 789 + silicone oil products; 2. Test method: The above-mentioned water-repellent and quick-drying agents were diluted with car wash liquid at a concentration of 0.3%, and the traditional amino silicone oil product was diluted with a concentration of 0.5% to obtain car wash liquids 1 to 11. The above products were tested for low-temperature stability according to GB / T16497-2007 (Determination of storage stability of water-in-oil emulsions of surfactants): The above products were mixed with sodium dodecylbenzenesulfonate at a volume ratio of 1:1. Then, 100 mL of each sample was placed at -5℃ and allowed to stand for 24 h to observe whether stratification occurred. At the same time, another 100 mL of each sample was placed at -10℃ and allowed to stand for 7 days to observe the flocculation state of the samples.

[0051] Meanwhile, the high-temperature stability of the samples in Examples 1 to 5 of this invention was tested according to the stability test in accordance with GB / T16497-2007.

[0052] The core parameters are as follows: Temperature: 50℃±2℃. Time: 24h, 72h, 168h (7 days).

[0053] Sample volume: 100 mL / sample (consistent with the low-temperature test, using sodium dodecylbenzenesulfonate at a 1:1 ratio). Preheating: Heat the oven to the target temperature of 50°C and stabilize for 30 min; Place the sample: Place the sample vials vertically in the center of the oven, avoiding stacking, and ensure hot air circulation.

[0054] Constant temperature exposure: After the set time is reached, remove the product and cool it to room temperature (25°C).

[0055] Observation Record: Layering: Whether oil / water phase separation occurs (interface clarity).

[0056] Flocculation / precipitation: Particulate matter or suspended flocculent matter at the bottom of the bottle.

[0057] 3. Experimental results: The specific experimental results are shown in Tables 2 and 3.

[0058] Table 2 Low-temperature stability of different test samples

[0059] Table 3 High-temperature stability of different test samples

[0060] As shown in Table 2 above, the samples of Examples 1-5 of this invention, thanks to the core synergistic system of Arquad 2C-75, XL-90, and G3H refined white oil, and the scientifically designed concentration range, exhibited excellent performance in low-temperature stability and anionic compatibility tests, fully meeting the practical application requirements of car wash products; in comparison: In Comparative Example 1, TX-10 was used instead of XL-90. Because the HLB value of TX-10 (13.5) was far from the 8-10 required by this invention, the hydrophilic segments were excessively combined with the aqueous phase at low temperatures, which disrupted the oil-water balance. In addition, its rigid structure containing benzene rings hindered the free movement of alkyl chains at low temperatures, which caused crystallization. At the same time, after mixing with anionic components, the microemulsion became turbid and precipitated. Finally, it completely separated at -10℃ and could not be restored to homogeneity. Its low-temperature stability and compatibility were completely unstable. In Comparative Example 2, Arquad 2C-75 was replaced with polyquaternium-2. This component has a simple alkyl chain structure, weak interfacial activity, poor synergy with G3H white oil, and its molecular arrangement is disordered and prone to crystallization at low temperatures. Moreover, its charge density does not match that of the anionic component, and local charge neutralization occurs during mixing, causing slight flocculation. Finally, precipitation occurs when mixed at -5℃, and it precipitates after 3 days at -10℃ and completely decomposes and becomes unstable after 7 days. In Comparative Example 3, the concentration of Arquad 2C-75 was reduced to 8%, which is lower than the 10-20% protection range of this invention. The insufficient concentration of the core cation prevented the formation of a dense interfacial film, resulting in a decrease in the emulsification stability of the microemulsion. The synergistic regulatory effect with XL-90 was weakened, the HLB value deviated from the optimal range, and no precipitation was observed when mixed at -5℃, but the system was slightly turbid. After standing at -10℃, the transparency of the microemulsion decreased significantly. Comparative Example 4 increased the Arquad 2C-75 concentration to 25%, which exceeded the scope of protection of this invention. The excessively high cation concentration led to an excessively high charge density, and when mixed with the anionic component, local charge neutralization caused flocculent precipitation. The excessive component also competed with XL-90 for adsorption, which interfered with the microemulsion interface structure and caused a decrease in oil phase compatibility, ultimately resulting in slight oil separation. There was no performance gain and the raw material was wasted. In the five comparative groups, after removing the necessary component XL-90, the HLB value of the system dropped to 5.2, which is far below the range required for water-in-oil microemulsions. The oil phase and water phase could not be effectively emulsified and directly separated. Moreover, without the low-temperature stability and resistance to Ostwald ripening of XL-90, the emulsion particles rapidly aggregated and crystallized at 5°C. After mixing with the anionic components, the floating oil was obvious, and the system completely separated and became unstable at -10°C. Traditional amino silicone oil formulations are ineffective because amino silicone oil molecules are highly rigid and have a high pour point, making them prone to crystallization at temperatures below -5°C. Their compatibility with the HLB values ​​of their associated emulsion systems is poor, further exacerbating oil-water separation at low temperatures. After standing at -10°C, they become completely unstable and irreversible. Furthermore, amino silicone oil is a cationic polymer, which undergoes a strong charge neutralization reaction when mixed with anionic sodium dodecylbenzenesulfonate, directly initiating flocculation and separation. It also easily forms difficult-to-remove silicone spots. Both its low-temperature stability and anionic compatibility have inherent defects, failing to meet practical application requirements.

[0061] Meanwhile, the high-temperature test results in Table 3 further demonstrate that the product of this invention also exhibits stability at a high temperature of 50°C.

[0062] Experiment Example 3: Practical Application Test 1. Test samples: Water-repellent and quick-drying agents prepared in Examples 1-5 and Comparative Examples 1-5, and traditional amino silicone oil water-repellent and quick-drying agents; 2. Experimental Procedure: The water-repellent and quick-drying agents of Examples 1-3 of this invention were diluted to a concentration of 0.3%, and the traditional amino silicone oil water-repellent and quick-drying agent was diluted to a concentration of 0.5% to obtain car wash liquids. Since there is no specific standard for water-repellent agents, the drying time was determined by Method A of surface drying time in GB / T1728-2020 (Determination of Drying Time of Paint Film and Putty Film) (in this experiment, the surface of the car after washing was used instead of the paint film surface). The gloss of the car after cleaning with the cleaning liquid was measured at 60° using an LS190 gloss meter. At the same time, the water droplets on the lotus leaves still fell off after rinsing with clean water after being cleaned and naturally dried with the cleaning liquid of this invention, which proved that it had a water-repellent effect, was used to test the durability of the cleaning liquid.

[0063] 3. Experimental results: The specific experimental results are shown in Table 4.

[0064] Table 4 Comparison of the practical applications of the present invention and traditional amino silicone oil formulations

[0065] As shown in Table 4 above, the cationic microemulsion water-repellent quick-drying agent prepared in Examples 1-5 of this invention is significantly superior to the comparative examples and traditional amino silicone oil products in terms of drying time, gloss, and durability. The drying time is only 12-13 minutes, which is nearly half that of traditional products. The gloss reaches 86-88 GU, an increase of 8-10 GU, and it still maintains a good water-repellent effect after 10 car washes. In contrast, comparative examples 1-5 have slower drying speed, reduced gloss, and significantly decreased durability due to surfactant replacement, improper concentration of core cationic components, or lack of key emulsifiers. Among them, comparative example 5 has the worst performance due to the lack of surfactant, with a drying time as long as 25 minutes, and it basically loses its water-repellent effect after 6 car washes. Traditional amino silicone oil products dry slowly and have low gloss. The water-repellent effect gradually deteriorates after only 7 car washes. The overall performance is far inferior to the product of this invention, which fully demonstrates that this invention achieves a synergistic improvement in quick-drying, gloss enhancement, and durability through reasonable component compounding and ratio design.

[0066] Further testing using GB38508-2020 determined the VOCs content of the car wash liquid of this invention, which met the limit requirements. Therefore, compared with the traditional amino silicone oil system, it achieves a comprehensive improvement in performance and significantly exceeds the standard benchmark, possessing superior practical application value.

[0067] It should be noted that the above-described embodiments should be understood as illustrative, not as limiting the scope of protection of this invention. The scope of protection of this invention is defined by the claims. For those skilled in the art, some non-essential improvements and adjustments made to this invention without departing from the essence and scope of this invention still fall within the scope of protection of this invention.

Claims

1. A cationic microemulsion water-repellent and quick-drying agent, characterized in that, It includes the following components and their mass percentages: 10-20% biscocarbamate dimethylammonium chloride, 5-10% isomeric decayl alcohol polyoxyethylene ether, 1-5% coupling agent, 25-35% refined white oil, and the balance being deionized water.

2. The cationic microemulsion water-repellent and quick-drying agent as described in claim 1, characterized in that, It includes the following components and their mass percentages: 13-18% biscocarbamate dimethylammonium chloride, 6-8% isomeric decayl alcohol polyoxyethylene ether, 2-4% coupling agent, 28-32% refined white oil, and the balance being deionized water.

3. The cationic microemulsion water-repellent and quick-drying agent as described in claim 2, characterized in that, It consists of the following components and their mass percentages: 15% biscocarbamate dimethylammonium chloride, 7% isomeric decayl alcohol polyoxyethylene ether, 3% coupling agent, 30% refined white oil, and the balance being deionized water.

4. The cationic microemulsion water-repellent and quick-drying agent according to any one of claims 1 to 3, characterized in that, The coupling agent is ethylene glycol butyl ether.

5. The cationic microemulsion water-repellent and quick-drying agent according to any one of claims 1 to 3, characterized in that, The refined white oil is an isoparaffin with a flash point of 135~140℃ and a purity of ≥99.5%; the deionized water has a mineralization of ≤50mg / L.

6. A method for preparing a cationic microemulsion water-repellent and quick-drying agent as described in any one of claims 1 to 5, characterized in that, The process includes the following: S1. Oil phase mixing: Heat the refined white oil to 38~45℃, then add the coupling agent and stir until transparent to obtain solution I; S2, Aqueous phase preparation: Add biscocarbamate dimethylammonium chloride and isomeric decayl alcohol polyoxyethylene ether to deionized water, stir in a water bath until uniformly mixed, to obtain solution II; S3. Pre-emulsification: Solution II obtained in step S2 is added dropwise to solution I obtained in step S1 at a rate of 1~3 mL / min, and a high-speed shear machine is turned on simultaneously to emulsify and form a pre-emulsion. S4. High-pressure homogenization: The pre-emulsion obtained in step S3 is transferred to a high-pressure homogenizer for homogenization to obtain a semi-transparent microemulsion. S5. Post-processing: The semi-transparent microemulsion obtained in step S4 is filtered through a sieve at 24~28℃ to obtain the final product.

7. The preparation method according to claim 6, characterized in that, The conditions for stirring until transparent in step S1 are to stir at a speed of 200~400 rpm for 10~15 min; the conditions for stirring in a water bath until uniformly mixed in step S2 are to stir in a water bath at 40~50℃ for 10~20 min.

8. The preparation method according to claim 6, characterized in that, During emulsification in step S3, the rotation speed is 7000~9000 rpm and the emulsification time is 10~15 min; the homogenization conditions in step S4 are to cycle homogenize 3~5 times under a pressure of 45~55 MPa and control the particle size to be 100~200 nm.

9. The use of a cationic microemulsion water-repellent quick-drying agent as described in any one of claims 1 to 5 in the preparation of car wash products.

10. A car wash product, characterized in that, The product includes the cationic microemulsion water-repellent and quick-drying agent according to any one of claims 1 to 5, wherein the mass percentage of the cationic microemulsion water-repellent and quick-drying agent is 0.1% to 0.3%.

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