Preparation method and application of anti-fouling anti-slip agent

By adding a specific proportion of nanotitanium dioxide, nanosilicon dioxide and triethanolamine to the anti-slip agent, as well as modified silicone oil and glycerin, anti-fouling and anti-slip agents, the problem of poor anti-fouling ability of existing anti-slip agents is solved, and higher anti-slip performance and wider application prospects are achieved.

CN119823718APending Publication Date: 2025-04-15SHANGHAI GREENHAOJI ENVIRONMENTAL PROTECTION TECHNOLOGY CO LTD
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Patent Information

Application Number
CN202510014899.0
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-01-06
Publication Date
2025-04-15

AI Technical Summary

Technical Problem

The existing anti-slip agent has poor anti-fouling ability and is easily worn. Oxalic acid in the raw materials is highly toxic and causes pollution to groundwater. It has a single purpose, poor stain resistance, easy to remain stains, and poor stability to cold and heat cycles.

Method used

The anti-fouling anti-fouling agent is added to deionized water in sequence, and after stirring evenly, the moisturizer, acid agent and antioxidant are added to prepare an anti-fouling anti-fouling agent. The antifouling composition consists of nanotitanium dioxide, nanosilica and triethanolamine, the anti-slip active agent is prepared from high hydrogen-containing silicone oil, cyclosiloxane and methyl methacrylate, and the moisturizing agent is prepared from glycerin, modified silicone oil and sodium lactate.

Benefits of technology

It improves the anti-fouling self-cleaning, anti-static, anti-bacterial, anti-ultraviolet, etc. properties of anti-fouling and anti-fouling agents, enhances the anti-slip and anti-fouling ability, extends the service life, and improves the water retention and anti-oxidation ability of the ceramic tile surface.

✦ Generated by Eureka AI based on patent content.

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Abstract

The invention relates to the technical field of anti-slip products, in particular to a preparation method and application of an anti-fouling anti-slip agent.The preparation method comprises the steps that a dispersing agent, an anti-slip active agent and an anti-fouling composition are sequentially added into deionized water, and pre-dispersion liquid is obtained after uniform stirring; adding a humectant into the pre-dispersion liquid, stirring, sequentially adding a combined acid agent and an antioxidant, and uniformly stirring to obtain the anti-fouling and anti-slip agent. Wherein the anti-skid active agent is prepared from high-hydrogen-content silicone oil, dimethyl mixed cyclosiloxane, methyl methacrylate and methylbenzene, the anti-skid capability can be improved, and meanwhile the anti-pollution capability of the anti-pollution anti-skid agent can be further improved; the humectant is obtained by mixing glycerol, modified silicone oil and sodium lactate, can improve the water retention capacity of the anti-fouling and anti-slip agent, and can also be matched with the antioxidant to improve the antioxidant capacity of the anti-fouling and anti-slip agent; the self-made anti-skid active agent is added. Therefore, the anti-pollution and anti-skid floor has higher anti-pollution capacity and anti-skid capacity and wider application prospect.
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Description

Technical Field

[0001] The invention relates to the technical field of anti-skid products, and in particular to a preparation method of an anti-fouling and anti-skid agent and application thereof. Background Art

[0002] More and more buildings use bright hard materials such as marble, tiles, and mosaics. These materials are indispensable for hospitals, schools, exhibition halls, hotels, supermarkets, shopping centers, restaurants, gymnasiums, swimming pools, and kitchens. However, the problem that follows is that slipping accidents continue to occur due to the smoothness of the ground, and even cause human disability. Among them, young children, the elderly, pregnant women, and people with limited mobility are the most serious, so ground anti-slip has become a major issue of public safety.

[0003] In order to make the floor anti-slip, one method is to make the floor into a macroscopic uneven structure, and use this structure and the mechanical bite effect of the sole under pressure to increase the friction coefficient. However, this method destroys the decorative effect of the floor, and has high requirements for the processing method, which increases the difficulty of tile processing. Another method is to apply an anti-slip agent on the floor, and use the anti-slip agent attached to the floor to increase the friction coefficient. Therefore, anti-slip agents have been widely studied and reported, such as the patent technical document CN109536135B discloses an anti-fouling and anti-slip agent for marble floor tiles and its preparation method. The invention includes the following components: 0.1-3 parts of an acid with a pKa of 2-4; 1-5 parts of a fluoride salt; 0.05-4 parts of a non-ionic surfactant; 0.1-2 parts of a brightener; 0.1-3 parts of an additive; and 80-100 parts of water. The acid with a pKa of 2-4 is composed of nitric acid, hydrofluoric acid, and citric acid.

[0004] However, these existing anti-slip agents still have the following disadvantages: the anti-slip agent layer will gradually wear out and lose its anti-slip effect as the use time increases; the main raw materials of anti-slip agent products are oxalic acid and hydrofluoric acid, oxalic acid is highly toxic and will cause serious pollution to groundwater; the use of anti-slip agents is relatively single, and some anti-slip agents are only suitable for indoor floors; the stain resistance is relatively poor, and it is easy to leave stains, it is not easy to clean, and the stability of resistance to cold and hot cycles is poor.

[0005] Therefore, according to the above-mentioned related technologies, it is urgent to develop a preparation method and application of an anti-fouling and anti-slip agent. Summary of the invention

[0006] In view of this, the purpose of the present invention is to provide a preparation method of an anti-fouling and anti-skid agent and its application, so as to solve the problem that the anti-fouling ability of the anti-skid agent prepared in the prior art is poor.

[0007] Based on the above purpose, the present invention provides a preparation method of an anti-fouling and anti-slip agent and its application.

[0008] A method for preparing an anti-fouling and anti-skid agent, characterized in that it comprises the following steps:

[0009] Step S1: adding a dispersant, an anti-skid active agent, and an anti-fouling composition to deionized water in sequence, and stirring evenly to obtain a pre-dispersed liquid;

[0010] Step S2: adding a moisturizer to the pre-dispersed liquid, stirring at 800-1000 rpm for 5-10 minutes, then sequentially adding a combined acid and an antioxidant, and stirring evenly to obtain an anti-fouling and anti-slip agent;

[0011] The anti-slip active agent in step S1 is prepared from high hydrogen silicone oil, dimethyl mixed cyclosiloxane, methyl methacrylate and toluene;

[0012] The antifouling composition in step S1 is obtained by mixing nano titanium dioxide, nano silicon dioxide and triethanolamine;

[0013] The moisturizing agent in step S2 is obtained by mixing glycerin, modified silicone oil and sodium lactate;

[0014] The modified silicone oil is prepared from silicone oil, N-(2-hydroxyethyl)piperazine and allyl polyether;

[0015] The combined acid agent in step S2 is any one or more of lactic acid and citric acid;

[0016] The antioxidant in step S2 is any one of sodium citrate and di-tert-butyl-p-cresol.

[0017] Preferably, the dispersant in step S1 is any one of polyethylene glycol, ethylene glycol amine, and sodium dodecyl sulfate.

[0018] Preferably, the preparation method of the anti-slip active agent in step S1 is as follows:

[0019] The polyvinyl alcohol and methyl cellulose are mixed and stirred at 600-800 rpm for 30-50 minutes, and then water-soluble starch and fatty alcohol polyoxyethylene are added in sequence, and then stirred evenly to obtain an anti-slip active agent.

[0020] Preferably, the mass ratio of the polyvinyl alcohol, methyl cellulose, water-soluble starch and fatty alcohol polyoxyethylene ether is 0.1-0.5:0.5-1:0.15-0.5:0.25-1.

[0021] Preferably, the mass ratio of the nano-titanium dioxide, nano-silicon dioxide and triethanolamine is 1-2:1-3:3.

[0022] Preferably, the mass ratio of the glycerol, modified silicone oil and sodium lactate is 1-2:3-5:1.

[0023] Preferably, the preparation method of the modified silicone oil is as follows:

[0024] Step A1: Add dimethyl mixed cyclosiloxane and hexamethyldisiloxane to high hydrogen silicone oil, heat to 70-75° C. in a constant temperature water bath, add a solid acid catalyst, stir the reaction for 4-6 hours, then cool to room temperature, filter to remove solid matter, and then distill the filtrate under reduced pressure to remove low boiling points to obtain low hydrogen silicone oil;

[0025] Step A2: adding methyl methacrylate, toluene and isopropanol solution of chloroplatinic acid to low hydrogen silicone oil, heating and stirring, heating to 80-85° C. and stirring at a constant temperature for 10-12 hours; removing toluene and methyl methacrylate by vacuum distillation, dissolving in ethanol, centrifuging and filtering to remove precipitates, and further distilling to remove ethanol to obtain modified silicone oil.

[0026] Preferably, the mass ratio of the high hydrogen silicone oil, dimethyl mixed cyclosiloxane, hexamethyldisiloxane and solid acid catalyst in step A1 is 25-27:20:0.8-1:2-3;

[0027] The amount ratio of the low hydrogen silicone oil, methyl methacrylate, toluene, and chloroplatinic acid isopropanol solution in step A2 is 10-20 g: 11-22 g: 8-13 g: 0.25-0.5 mL;

[0028] The mass fraction of the chloroplatinic acid solution in step A2 is 0.5%.

[0029] Preferably, the mass ratio of the deionized water, the dispersant, the anti-slip active agent, the anti-fouling composition, the moisturizing agent, the combined acid agent, and the antioxidant is 50-60:20-25:1-3:5-8:5-8:1-4:1-5.

[0030] An application of anti-fouling and anti-slip agent, which can be applied to tiles in supermarkets, kitchens, swimming pools, bathrooms, and hospitals

[0031] Beneficial effects of the present invention:

[0032] The present invention provides a method for preparing an anti-fouling and anti-skid agent and its application. The present invention effectively improves the anti-fouling and self-cleaning, antistatic, antibacterial, anti-ultraviolet and other properties of the anti-fouling and anti-skid agent by adding nano titanium dioxide, nano silicon dioxide and triethanolamine compounded in a specific ratio; the addition of the self-made anti-skid active agent of the present invention can improve the anti-skid ability and further improve the anti-fouling ability of the anti-fouling and anti-skid agent; the addition of a moisturizer prepared by glycerol, modified silicone oil and sodium lactate in a specific ratio can not only improve the water retention capacity of the anti-fouling and anti-skid agent, but also cooperate with an antioxidant to improve its antioxidant capacity. Therefore, compared with the prior art, the anti-fouling and anti-skid agent prepared by the present invention has higher anti-fouling ability, anti-skid ability and wider application prospects. DETAILED DESCRIPTION

[0033] In order to make the objectives, technical solutions and advantages of the present invention more clearly understood, the present invention is further described in detail below in conjunction with specific embodiments.

[0034] Example 1: A method for preparing an anti-fouling and anti-slip agent is as follows:

[0035] S1: Add 20g of dimethyl mixed cyclosiloxane and 0.8g of hexamethyldisiloxane to 25g of high hydrogen silicone oil, heat to 70°C in a constant temperature water bath, add 2g of solid acid catalyst, stir and react for 4h, then cool to room temperature, filter to remove solid matter, and then distill the filtrate under reduced pressure to remove low boiling points to obtain low hydrogen silicone oil;

[0036] S2: Add 11 g of methyl methacrylate, 8 g of toluene and 0.25 mL of 0.5% chloroplatinic acid isopropanol solution to 10 g of low-hydrogen silicone oil, heat and stir, heat to 805° C. and stir at constant temperature for 10 h; remove toluene and methyl methacrylate by vacuum distillation, dissolve in ethanol, centrifuge and filter to remove precipitate, and then distill to remove ethanol to obtain modified silicone oil;

[0037] S3: 1 g of glycerol, 3 g of modified silicone oil, and 1 g of sodium lactate were mixed evenly to obtain a moisturizer;

[0038] S4: 0.1 g of polyvinyl alcohol and 0.5 g of methyl cellulose were mixed and stirred at 600 rpm for 30 min, and then 0.15 g of water-soluble starch and 0.25 g of fatty alcohol polyoxyethylene were added in sequence, and then stirred evenly to obtain an anti-slip active agent;

[0039] S5: Evenly mix 1 g of nano titanium dioxide, 1 g of nano silicon dioxide, and 3 g of triethanolamine to obtain an antifouling composition;

[0040] S6: Add 20 g of polyethylene glycol, 1 g of an anti-slip active agent, and 5 g of an anti-fouling composition to 50 g of deionized water in sequence, and stir evenly to obtain a pre-dispersion liquid;

[0041] S7: Add 5 g of moisturizer to 76 g of the pre-dispersion liquid, stir at 800 rpm for 5 min, then add 1 g of lactic acid and 1 g of sodium citrate in sequence, and stir evenly to obtain an anti-fouling and anti-slip agent;

[0042] Example 2: A method for preparing an anti-fouling and anti-slip agent is as follows:

[0043] S1: Add 20g of dimethyl mixed cyclosiloxane and 0.9g of hexamethyldisiloxane to 25.5g of high hydrogen silicone oil, heat to 72°C in a constant temperature water bath, add 2.3g of solid acid catalyst, stir and react for 4.5h, then cool to room temperature, filter to remove solid matter, and then distill the filtrate under reduced pressure to remove low boiling points to obtain low hydrogen silicone oil;

[0044] S2: Add 15 g of methyl methacrylate, 10 g of toluene and 0.3 mL of 0.5% chloroplatinic acid isopropanol solution to 13 g of low-hydrogen silicone oil, and heat while stirring. Heat to 82° C. and stir at constant temperature for 10.5 h. Distill under reduced pressure to remove toluene and methyl methacrylate, and then dissolve in ethanol. Centrifuge and filter to remove precipitate, and then distill to remove ethanol to obtain modified silicone oil.

[0045] S3: 1.5 g of glycerol, 3.5 g of modified silicone oil, and 1 g of sodium lactate were mixed evenly to obtain a moisturizer;

[0046] S4: 0.2 g of polyvinyl alcohol and 0.7 g of methyl cellulose were mixed and stirred at 650 rpm for 35 min, and 0.2 g of water-soluble starch and 0.5 g of fatty alcohol polyoxyethylene were added in sequence, and then stirred evenly to obtain an anti-slip active agent;

[0047] S5: 1.3 g of nano titanium dioxide, 1.3 g of nano silicon dioxide, and 3 g of triethanolamine are mixed evenly to obtain an antifouling composition;

[0048] S6: Add 22 g of ethylene glycol amine, 1.4 g of anti-skid active agent, and 5.6 g of anti-fouling composition to 53 g of deionized water in sequence, and stir evenly to obtain a pre-dispersion liquid;

[0049] S7: Add 6 g of moisturizing agent to 82 g of pre-dispersion liquid, stir at 850 rpm for 7 min, then add 2 g of citric acid and 2 g of sodium citrate in sequence, and stir evenly to obtain an anti-fouling and anti-slip agent;

[0050] Example 3: A method for preparing an anti-fouling and anti-slip agent is as follows:

[0051] S1: Add 20g of dimethyl mixed cyclosiloxane and 0.9g of hexamethyldisiloxane to 26g of high hydrogen silicone oil, heat to 73°C in a constant temperature water bath, add 2.5g of solid acid catalyst, stir and react for 5h, then cool to room temperature, filter to remove solid matter, and then distill the filtrate under reduced pressure to remove low boiling points to obtain low hydrogen silicone oil;

[0052] S2: Add 18 g of methyl methacrylate, 11 g of toluene and 0.4 mL of 0.5% chloroplatinic acid isopropanol solution to 17 g of low hydrogen silicone oil, and heat while stirring. Heat to 84° C. and stir at constant temperature for 11 h. Distill under reduced pressure to remove toluene and methyl methacrylate, and then dissolve in ethanol. Centrifuge and filter to remove precipitate, and then distill to remove ethanol to obtain modified silicone oil.

[0053] S3: 1.8 g of glycerol, 4.2 g of modified silicone oil, and 1 g of sodium lactate were mixed evenly to obtain a moisturizer;

[0054] S4: 0.4 g of polyvinyl alcohol and 0.9 g of methyl cellulose were mixed and stirred at 700 rpm for 40 min, and 0.4 g of water-soluble starch and 0.8 g of fatty alcohol polyoxyethylene were added in sequence, and then stirred evenly to obtain an anti-slip active agent;

[0055] S5: 1.8 g of nano titanium dioxide, 1.7 g of nano silicon dioxide, and 3 g of triethanolamine are mixed evenly to obtain an antifouling composition;

[0056] S6: Add 23 g of sodium dodecyl sulfate, 2.5 g of anti-skid active agent, and 6.5 g of anti-fouling composition to 58 g of deionized water in sequence, and stir evenly to obtain a pre-dispersion liquid;

[0057] S7: Add 7 g of moisturizer to 90 g of the pre-dispersion liquid, stir at 900 rpm for 8 min, then add 2 g of lactic acid, 1 g of citric acid and 3 g of sodium citrate in sequence, and stir evenly to obtain an anti-fouling and anti-slip agent;

[0058] Example 4: A method for preparing an anti-fouling and anti-slip agent is as follows:

[0059] S1: Add 20g of dimethyl mixed cyclosiloxane and 1g of hexamethyldisiloxane to 27g of high hydrogen silicone oil, heat to 75°C in a constant temperature water bath, add 3g of solid acid catalyst, stir and react for 6h, then cool to room temperature, filter to remove solid matter, and then distill the filtrate under reduced pressure to remove low boiling points to obtain low hydrogen silicone oil;

[0060] S2: Add 22g of methyl methacrylate, 13g of toluene and 0.5mL of 0.5% chloroplatinic acid isopropanol solution to 20g of low hydrogen silicone oil, and heat while stirring. Heat to 85°C and stir at constant temperature for 12h; remove toluene and methyl methacrylate by vacuum distillation, dissolve in ethanol, centrifuge and filter to remove precipitate, and then distill to remove ethanol to obtain modified silicone oil;

[0061] S3: 2 g of glycerol, 5 g of modified silicone oil, and 1 g of sodium lactate were mixed evenly to obtain a moisturizer;

[0062] S4: 0.5 g of polyvinyl alcohol and 1 g of methyl cellulose were mixed and stirred at 800 rpm for 50 min, and then 0.5 g of water-soluble starch and 1 g of fatty alcohol polyoxyethylene were added in sequence, and then stirred evenly to obtain an anti-slip active agent;

[0063] S5: 2 g of nano titanium dioxide, 3 g of nano silicon dioxide, and 3 g of triethanolamine are mixed evenly to obtain an antifouling composition;

[0064] S6: Add 25 g of polyethylene glycol, 3 g of anti-slip active agent, and 8 g of anti-fouling composition to 60 g of deionized water in sequence, and stir evenly to obtain a pre-dispersion liquid;

[0065] S7: Add 8 g of moisturizer to 96 g of the pre-dispersion liquid, stir at 1000 rpm for 10 min, then add 2 g of lactic acid, 2 g of citric acid and 5 g of di-tert-butyl-p-cresol in sequence, and stir evenly to obtain an anti-fouling and anti-slip agent;

[0066] Comparative Example 1:

[0067] Compared with Example 1, this comparative example did not add in the preparation process, and the other steps and parameters were the same, which will not be repeated in this comparative example, and finally an anti-fouling and anti-skid agent was obtained.

[0068] Comparative Example 1:

[0069] Compared with Example 1, this comparative example only replaces the "1g glycerin, 3g modified silicone oil, 1g sodium lactate" added in the preparation process of the moisturizer with "5g glycerin", and the remaining steps and parameters are the same, which will not be repeated in this comparative example, and finally an anti-fouling and anti-slip agent is obtained.

[0070] Comparative Example 2:

[0071] Compared with Example 1, this comparative example only replaces the "1g glycerin, 3g modified silicone oil, 1g sodium lactate" added in the preparation process of the moisturizer with "2g glycerin, 3g modified silicone oil", and the remaining steps and parameters are the same. This comparative example will not be repeated, and finally an anti-fouling and anti-slip agent is obtained.

[0072] Comparative Example 3:

[0073] Compared with Example 1, this comparative example only replaces the "1g anti-slip active agent" added in the preparation process of the anti-fouling and anti-skid agent with "1g non-ionic surfactant (fatty alcohol polyoxyethylene ether)", and the remaining steps and parameters are the same, which will not be repeated in this comparative example, and finally the anti-fouling and anti-skid agent is obtained.

[0074] Comparative Example 4:

[0075] Compared with Example 1, this comparative example only replaces the "1g nano-titanium dioxide, 1g nano-silicon dioxide, 3g triethanolamine" added in the preparation process of the anti-fouling composition with "5g nano-titanium dioxide", and the remaining steps and parameters are the same, which will not be repeated in this comparative example, and finally an anti-fouling and anti-slip agent is obtained.

[0076] Comparative Example 5:

[0077] Compared with Example 1, this comparative example only replaces the "1g nano-titanium dioxide, 1g nano-silicon dioxide, 3g triethanolamine" added in the preparation process of the anti-fouling composition with "5g triethanolamine", and the remaining steps and parameters are the same, which will not be repeated in this comparative example, and finally an anti-fouling and anti-slip agent is obtained.

[0078] Comparative Example 6: A method for preparing an anti-fouling and anti-slip agent is as follows:

[0079] S1: Add 20g of dimethyl mixed cyclosiloxane and 0.8g of hexamethyldisiloxane to 25g of high hydrogen silicone oil, heat to 70°C in a constant temperature water bath, add 2g of solid acid catalyst, stir and react for 4h, then cool to room temperature, filter to remove solid matter, and then distill the filtrate under reduced pressure to remove low boiling points to obtain low hydrogen silicone oil;

[0080] S2: Add 11 g of methyl methacrylate, 8 g of toluene and 0.25 mL of 0.5% chloroplatinic acid isopropanol solution to 10 g of low-hydrogen silicone oil, heat and stir, heat to 805° C. and stir at constant temperature for 10 h; remove toluene and methyl methacrylate by vacuum distillation, dissolve in ethanol, centrifuge and filter to remove precipitate, and then distill to remove ethanol to obtain modified silicone oil;

[0081] S3: 1 g of glycerol, 3 g of modified silicone oil, and 1 g of sodium lactate were mixed evenly to obtain a moisturizer;

[0082] S4: 0.1 g of polyvinyl alcohol and 0.5 g of methyl cellulose were mixed and stirred at 600 rpm for 30 min, and then 0.15 g of water-soluble starch and 0.25 g of fatty alcohol polyoxyethylene were added in sequence, and then stirred evenly to obtain an anti-slip active agent;

[0083] S5: Evenly mix 1 g of nano titanium dioxide, 1 g of nano silicon dioxide, and 3 g of triethanolamine to obtain an antifouling composition;

[0084] S6: adding 20 g of polyethylene glycol, 1 g of an anti-slip active agent, 5 g of an anti-fouling composition, 5 g of a moisturizer, 1 g of lactic acid and 1 g of sodium citrate to 50 g of deionized water, and stirring evenly to obtain an anti-fouling and anti-slip agent;

[0085] Performance Test:

[0086] Friction coefficient test:

[0087] Referring to the test standard of JC / T1050-2007 "Classification and Test Methods of Anti-slip Performance of Floor Stone", the friction coefficient of Marco Polo tiles was tested in dry state, wet state and 12 months after dry treatment. The size of the floor tile is 150mm×150mm×5mm; the dry state is to dry the marble floor tile treated with anti-fouling and anti-slip agent at 30℃ for 60 minutes; the wet state is that the water content on the surface of the marble floor tile is ≥0.1mm. The calculation method of the friction coefficient retention rate after 12 months: the initial tile friction coefficient is recorded as A1, and the tile friction coefficient after 12 months is recorded as A2; the test results are shown in Table 1; the friction coefficient retention rate calculation formula is as follows;

[0088]

[0089] Gloss test:

[0090] The gloss meter model WGG60-E4 produced by Koshijia Optoelectronic Instrument Co., Ltd. was used to test the gloss of the tiles treated with anti-fouling and anti-slip agents in the dry state and the gloss retention rate after 12 months; the initial gloss was recorded as B1, and the gloss after 12 months was recorded as B2; the test results are shown in Table 1; the gloss retention rate (%) is calculated as follows:

[0091]

[0092] Stability test:

[0093] According to the test standard of GB / T4893.7-2013 "Test for physical and chemical properties of furniture surface paint film Part 7: Determination of temperature difference between hot and cold temperatures", the stability of the hot and cold cycles of the tiles treated with the anti-fouling and anti-slip agents prepared in Examples 1 to 4 and Comparative Examples 1 to 6 was tested to observe whether there was cracking after 30 cycles. The test results are shown in Table 1;

[0094] Determination of antifouling ability:

[0095] The tiles were treated with the anti-fouling and anti-slip agents prepared in Examples 1 to 4 and Comparative Examples 1 to 6, and then immersed in ink containing 2 wt% ink at 25°C for 24 hours, and then placed at 25°C for 24 hours, and then immersed in pure water at 25°C for 1 hour and then taken out to observe the ink marks on the surface of the tiles treated with the anti-fouling and anti-slip agents prepared in Examples 1 to 4 and Comparative Examples 1 to 6. The measurement results are shown in Table 1;

[0096] Table 1

[0097]

[0098] Data Analysis:

[0099] As can be seen from Table 1, the anti-fouling and anti-skid agent prepared by the present invention has better anti-skid ability, anti-skid stability, gloss improvement ability and stability, freeze-thaw stability and anti-fouling ability;

[0100] This may be due to the specific proportion of nano titanium dioxide, nano silicon dioxide and triethanolamine added to the anti-fouling and anti-skid agent of the present invention, which effectively improves the anti-fouling, self-cleaning, antistatic, antibacterial, anti-ultraviolet and other properties of the anti-fouling and anti-skid agent; the hydrogen bonds of the polyvinyl alcohol in the homemade anti-skid active agent of the present invention and the hydroxyl groups on the methyl cellulose molecular chain can generate a multi-dimensional membrane with a three-dimensional structure, reducing the active hydroxyl group to improve the anti-skid ability, while the water-soluble starch and fatty alcohol polyoxyethylene can improve the freeze-thaw stability, anti-fouling ability and self-cleaning ability; therefore, the addition of the anti-skid active agent can improve the anti-skid ability and service life of the anti-skid agent, and can further improve the anti-fouling ability and self-cleaning ability of the anti-fouling and anti-skid agent. The invention modifies the high hydrogen silicone oil, and effectively improves the self-emulsification ability of the silicone oil, the centrifugal stability of the emulsion, the thermal stability, the low temperature stability, the freeze-thaw stability, and the acid, alkali and electrolyte resistance of the silicone oil; then, the silicone oil is compounded with glycerol with good water absorption and sodium lactate which can lock water by forming hydrogen bonds with water molecules in a specific ratio, so that a stable film integrating water absorption and water retention can be formed on the surface of the ceramic tile after being treated with the anti-fouling and anti-slip agent; therefore, the addition of a moisturizer prepared by glycerol, modified silicone oil and sodium lactate in a specific ratio can not only improve the water retention capacity of the anti-fouling and anti-slip agent, but also cooperate with an antioxidant to improve its antioxidant capacity.

[0101] Compared with Example 1, Comparative Example 1 only replaces "1g glycerol, 3g modified silicone oil, 1g sodium lactate" added in the preparation process of the moisturizer with "5g glycerol"; Compared with Example 1, Comparative Example 2 only replaces "1g glycerol, 3g modified silicone oil, 1g sodium lactate" added in the preparation process of the moisturizer with "2g glycerol, 3g modified silicone oil". It can be seen from Table 1 that compared with Example 1, the anti-skid ability, anti-skid stability, gloss improvement ability and stability, freeze-thaw stability and anti-fouling ability of Comparative Examples 1 and 2 are all reduced. This may be due to the modification of the high hydrogen silicone oil in the present invention. It effectively improves the self-emulsification ability of silicone oil, centrifugal stability of emulsion, thermal stability, low temperature stability, freeze-thaw stability, and acid, alkali and electrolyte resistance; then it is compounded with glycerol with good water absorption and sodium lactate that can lock water by forming hydrogen bonds with water molecules in a specific proportion, so that a stable film that combines water absorption and water retention can be formed on the surface of the tile after being treated with the anti-fouling and anti-slip agent; therefore, the addition of a moisturizer prepared by glycerol, modified silicone oil and sodium lactate in a specific proportion can not only improve the water retention capacity of the anti-fouling and anti-slip agent, but also cooperate with the antioxidant to improve its antioxidant capacity;

[0102] Comparative Example 3 Compared with Example 1, only the "1g anti-skid active agent" added in the preparation process of the anti-fouling and anti-skid agent is replaced with "1g non-ionic surfactant (fatty alcohol polyoxyethylene ether)". It can be seen from Table 1 that compared with Example 1, its anti-skid ability, anti-skid stability, gloss improvement ability and stability, and freeze-thaw stability are slightly reduced. This may be because compared with the non-ionic surfactant, the hydrogen bonds of the polyvinyl alcohol in the homemade anti-skid active agent of the present invention and the hydroxyl groups on the methyl cellulose molecular chain can generate a three-dimensional multi-dimensional membrane, reducing the active hydroxyl group, thereby improving the anti-skid ability, while the water-soluble starch and fatty alcohol polyoxyethylene can improve the freeze-thaw stability, anti-fouling ability and self-cleaning ability of the anti-skid active agent;

[0103] Compared with Example 1, Comparative Example 4 only replaces "1g nano titanium dioxide, 1g nano silicon dioxide, 3g triethanolamine" added in the preparation process of the antifouling composition with "5g nano titanium dioxide"; Compared with Example 1, Comparative Example 5 only replaces "1g nano titanium dioxide, 1g nano silicon dioxide, 3g triethanolamine" added in the preparation process of the antifouling composition with "5g triethanolamine"; It can be seen from Table 1 that compared with Example 1, the antifouling ability of Comparative Examples 4 and 5 is significantly reduced, which may be due to the specific proportion of nano titanium dioxide, nano silicon dioxide, and triethanolamine added to the antifouling and anti-skid agent of the present invention, which can effectively improve the antifouling, self-cleaning, antistatic, antibacterial, anti-ultraviolet and other properties of the antifouling and anti-skid agent;

[0104] In Comparative Example 6, during the preparation of the anti-fouling and anti-skid agent, the components are directly mixed and then stirred evenly. It can be seen from Table 1 that compared with the process of Example 1, "first, 22g of ethylene glycol amine, 1.4g of anti-skid active agent, and 5.6g of anti-fouling composition are added in sequence to 53g of deionized water, and the pre-dispersion liquid is obtained after stirring evenly; then, 6g of moisturizer is added to 82g of the pre-dispersion liquid, and the mixture is stirred at 850rpm for 7min, and then 2g of citric acid and 2g of sodium citrate are added in sequence, and the anti-fouling and anti-skid agent is obtained after stirring evenly.", the anti-skid ability, anti-skid stability, gloss improvement ability and stability, freeze-thaw stability and anti-fouling ability are all reduced. This may be because the present invention can generate the most ideal anti-fouling and anti-skid agent by mixing the reaction in a specific order, while directly mixing and stirring all the components will generate other by-products that affect the performance of the anti-fouling and anti-skid agent.

[0105] Those skilled in the art should understand that the discussion of any of the above embodiments is merely illustrative and is not intended to imply that the scope of the present invention is limited to these examples. Under the concept of the present invention, the technical features in the above embodiments or different embodiments may be combined, the steps may be implemented in any order, and there are many other variations of the different aspects of the present invention as described above, which are not provided in detail for the sake of simplicity.

[0106] The present invention is intended to cover all such substitutions, modifications and variations that fall within the broad scope of the appended claims. Therefore, any omissions, modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention should be included in the scope of protection of the present invention.

Claims

1. A method for preparing an anti-fouling and anti-slip agent, characterized in that: The following steps are involved: Step S1: adding a dispersant, an anti-slip active agent, and an anti-fouling composition to deionized water in sequence, and stirring evenly to obtain a pre-dispersed liquid; Step S2: adding a moisturizer to the pre-dispersed liquid, stirring at 800-1000 rpm for 5-10 min, then sequentially adding a combined acid and an antioxidant, and stirring evenly to obtain an anti-fouling and anti-slip agent; The anti-slip active agent in step S1 is prepared from high hydrogen silicone oil, dimethyl mixed cyclosiloxane, methyl methacrylate and toluene; The antifouling composition in step S1 is obtained by mixing nano titanium dioxide, nano silicon dioxide and triethanolamine; The moisturizing agent in step S2 is obtained by mixing glycerin, modified silicone oil and sodium lactate; The modified silicone oil is prepared from silicone oil, N-(2-hydroxyethyl)piperazine and allyl polyether; The combined acid agent in step S2 is any one or more of lactic acid and citric acid; The antioxidant in step S2 is any one of sodium citrate and di-tert-butyl-p-cresol.

2. The method for preparing the antifouling and antiskid agent according to claim 1, characterized in that: The dispersant in step S1 is any one of polyethylene glycol, ethylene glycol amine, and sodium dodecyl sulfate.

3. The method for preparing the anti-fouling and anti-skid agent according to claim 1, characterized in that: The preparation method of the anti-slip active agent in step S1 is as follows: The polyvinyl alcohol and methyl cellulose are mixed and stirred at 600-800 rpm for 30-50 minutes, and then water-soluble starch and fatty alcohol polyoxyethylene are added in sequence, and then stirred evenly to obtain an anti-slip active agent.

4. The method for preparing the anti-fouling and anti-skid agent according to claim 3, characterized in that: The mass ratio of the polyvinyl alcohol, methyl cellulose, water-soluble starch and fatty alcohol polyoxyethylene ether is 0.1-0.5:0.5-1:0.15-0.5:0.25-1.

5. The method for preparing the anti-fouling and anti-skid agent according to claim 1, characterized in that: The mass ratio of the nano titanium dioxide, nano silicon dioxide and triethanolamine is 1-2:1-3:

3.

6. The method for preparing the antifouling and antiskid agent according to claim 1, characterized in that: The mass ratio of the glycerol, modified silicone oil and sodium lactate is 1-2:3-5:

1.

7. The method for preparing the anti-fouling and anti-skid agent according to claim 1, characterized in that: The preparation method of the modified silicone oil is as follows: Step A1: Add dimethyl mixed cyclosiloxane and hexamethyldisiloxane to high hydrogen silicone oil, heat to 70-75° C. in a constant temperature water bath, add a solid acid catalyst, stir the reaction for 4-6 hours, then cool to room temperature, filter to remove solid matter, and then distill the filtrate under reduced pressure to remove low boiling points to obtain low hydrogen silicone oil; Step A2: adding methyl methacrylate, toluene and isopropanol solution of chloroplatinic acid to low hydrogen silicone oil, heating and stirring, heating to 80-85° C. and stirring at a constant temperature for 10-12 hours; removing toluene and methyl methacrylate by vacuum distillation, dissolving in ethanol, centrifuging and filtering to remove precipitates, and further distilling to remove ethanol to obtain modified silicone oil.

8. The method for preparing the antifouling and antiskid agent according to claim 7, characterized in that: The mass ratio of the high hydrogen silicone oil, dimethyl mixed cyclosiloxane, hexamethyldisiloxane and solid acid catalyst in step A1 is 25-27:20:0.8-1:2-3; The amount ratio of the low hydrogen silicone oil, methyl methacrylate, toluene, and chloroplatinic acid isopropanol solution in step A2 is 10-20 g: 11-22 g: 8-13 g: 0.25-0.5 mL; The mass fraction of the chloroplatinic acid solution in step A2 is 0.5%.

9. The method for preparing the anti-fouling and anti-skid agent according to claim 1, characterized in that: The mass ratio of the deionized water, the dispersant, the anti-skid active agent, the anti-fouling composition, the moisturizing agent, the combined acid agent and the antioxidant is 50-60:20-25:1-3:5-8:5-8:1-4:1-5.

10. Use of the anti-fouling and anti-slip agent according to any one of claims 1 to 9, characterized in that: It can be applied to tiles in supermarkets, kitchens, swimming pools, bathrooms and hospitals.

Citation Information

Patent Citations

  • A stain-resistant and anti-slip agent for marble floor tiles and its preparation method

    CN109536135B