A bio-based epoxy matte joint sealer and its preparation method

Abstract

The present application discloses a bio-based epoxy matte caulking agent and a preparation method thereof, relating to the technical field of bio-based caulking agents. The caulking agent comprises component A and component B. By mass parts, component A comprises: 75-85 parts of bio-based epoxy resin, 1-1.5 parts of dispersant, 1-1.5 parts of defoamer, 8-10 parts of compounded matte silica, 10-12 parts of hydrophobic fumed silica, and 5-10 parts of modified hollow glass microspheres; component B comprises: 70-80 parts of bio-based epoxy curing agent, 5-8 parts of hydrophobic fumed silica, 8-10 parts of compounded matte silica, 5-10 parts of modified hollow glass microspheres, and 5-7 parts of color paste; the bio-based epoxy resin is a phosphorus-containing itaconic acid-based epoxy resin; the bio-based epoxy curing agent is a phosphorus-containing cardanol-based curing agent. The caulking agent provided by the present application uses bio-based epoxy resin and curing agent, with more environmentally friendly components, less impact on the environment, and more remarkable matte degree, ultraviolet resistance, bonding strength, surface drying time, flame retardancy and antibacterial rate.

Description

Technical Field

[0001] The present application relates to the field of bio-based caulking agents, and in particular to a bio-based epoxy matte caulking agent and a preparation method thereof. Background Art

[0002] In order to prevent the thermal expansion and contraction of tiles, a gap is generally left during tiling. The filling of tile gaps has gradually evolved from products such as cement and colored caulking agents to reactive resin caulking agents (hereinafter referred to as "caulking agents"). Caulking agents are mainly paste-like caulking materials composed of polymers such as epoxy resin and polyurethane as the base material, added with various pigments, fillers and additives, and can play roles such as decoration, waterproofing, and mildew prevention. In recent years, caulking agents have been taken seriously and developed rapidly, and now they have become essential materials in the field of decoration and renovation. Current caulking agents have the advantages of antibacterial, mildew-proof, waterproof, non-discoloring, high gloss, and a variety of color types. They are high-end caulking materials developed in recent years and are widely applicable to the gap beautification of mosaics, tiles, stones, glass bricks, etc., and have gradually replaced white cement and caulking agents.

[0003] Although current caulking agent products have a wide variety of functions, they generally have the problem of high VOC. With the increasing demand for high-environmental products by people and the growing global attention to sustainable development and environmental protection, the development of bio-based caulking agents is particularly important. Bio-based caulking agents are prepared from renewable resources through innovative technologies. They not only inherit the advantages of traditional caulking agents in terms of yellowing resistance, moisture resistance and environmental protection, but also further improve the performance of the product such as adhesion and low toxicity by adding bio-based components. At the same time, the production process of bio-based caulking agents is more environmentally friendly, reducing the dependence on fossil resources and environmental pollution, and conforming to the development trend of future green building materials. Therefore, it is urgent to develop a green and environmentally friendly bio-based caulking agent with excellent functions to meet the urgent needs of the market for environmentally friendly and high-performance caulking products. Summary of the Invention

[0004] In order to provide a bio-based caulking agent product that is green, environmentally friendly and has excellent functions, the present application provides a bio-based epoxy matte caulking agent and a preparation method thereof.

[0005] The bio-based epoxy matte caulking agent and the preparation method thereof provided by the present application adopt the following technical solutions:

[0006] A bio-based epoxy matte caulking agent, comprising component A and component B;

[0007] By mass, the component A includes: 75-85 parts of bio-based epoxy resin, 1-1.5 parts of dispersant, 1-1.5 parts of defoamer, 8-10 parts of compounded matte silica, 10-12 parts of hydrophobic fumed silica, and 5-10 parts of modified hollow glass microspheres;

[0008] In terms of parts by mass, the component B includes: 70 - 80 parts of bio - based epoxy curing agent, 5 - 8 parts of hydrophobic fumed silica, 8 - 10 parts of compounded matting silica, 5 - 10 parts of modified hollow glass microspheres, and 5 - 7 parts of color paste.

[0009] By adopting the above - mentioned technical solution, using bio - based epoxy resin and bio - based epoxy curing agent as the key components of the caulking agent material, adding compounded matting silica, hydrophobic fumed silica, and modified hollow glass microspheres, the prepared caulking agent has good anti - ultraviolet performance, antibacterial and mildew - proof performance, flame - retardant performance, and has a matte texture. The material components are safe, the VOC emission is low, it is environmentally friendly, green, and the bonding force and strength of the product are high, ensuring a firm bond between the caulking agent and substrates such as tiles and stones, and it is not easy to fall off.

[0010] Preferably, the dispersant is BYK - 2155 type dispersant.

[0011] Preferably, the defoamer is Degussa 900 type defoamer.

[0012] Preferably, the compounded matting silica raw material includes 10 - 20% of Tosoh SS20 matting silica, 15 - 25% of Grace ED60 matting silica, 10 - 20% of Evonik TS100 matting silica, and 35% - 65% of Aerospace Saide 690 matting silica by mass percentage.

[0013] Preferably, the bio - based epoxy resin is phosphorus - containing itaconic acid - based epoxy resin; the phosphorus - containing itaconic acid - based epoxy resin is prepared from the following raw materials in parts by weight: 21.6 - 43.2 parts of 9,10 - dihydro - 9 - oxa - 10 - phosphaphenanthrene - 10 - oxide, 70 - 140 parts of xylene, 3 - 6 parts of catalyst, 13 - 26 parts of itaconic acid, 60 - 70 parts of acetone, 5.2 - 6.8 parts of epoxy bromopropane, and 5.8 - 7.2 parts of DBU.

[0014] Preferably, the bio - based epoxy curing agent is phosphorus - containing cardanol - based curing agent; the phosphorus - containing cardanol - based curing agent is prepared from the following raw materials in parts by weight: 10 - 20 parts of cardanol, 3 - 7 parts of triethylamine, 14 - 20 parts of chloroform, 9 - 18 parts of diphenyl chlorophosphate, 3.4 - 6.8 parts of diethylenetriamine, and 2.7 - 5.4 parts of formaldehyde solution.

[0015] Preferably, the modified hollow glass microsphere raw material includes alkali - treated hollow glass microspheres and chitosan acetate solution with a concentration of 1 - 5 g / L, and the solid - liquid ratio of the two is 1:8 - 14 g / mL.

[0016] This application also provides a preparation method of a bio - based epoxy matte caulking agent, adopting the following technical solution:

[0017] A preparation method of a bio-based epoxy matte caulking agent, comprising the following steps:

[0018] Mix 75 - 85 parts of bio-based epoxy resin, 1 - 1.5 parts of dispersant, 1 - 1.5 parts of defoamer, 8 - 10 parts of compounded matting silica, 10 - 12 parts of hydrophobic fumed silica, and 5 - 10 parts of modified hollow glass microspheres evenly by weight to obtain the component A; mix 70 - 80 parts of bio-based epoxy curing agent, 5 - 8 parts of hydrophobic fumed silica, 8 - 10 parts of compounded matting silica, 5 - 10 parts of modified hollow glass microspheres, and 5 - 7 parts of color paste evenly by weight to obtain the component B.

[0019] Preferably, the preparation method of the bio-based epoxy resin comprises the following steps:

[0020] Mix 21.6 - 43.2 parts of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, 70 - 140 parts of xylene, and 3 - 6 parts of catalyst evenly, heat to 120 - 140 °C, then dropwise add 13 - 26 parts of itaconic acid, react for 12 - 20 h, and obtain an intermediate product after the reaction; cool the intermediate product to room temperature, then filter, wash, and vacuum dry for 4 - 6 h, add the intermediate product to 60 - 70 parts of acetone, add 5.2 - 6.8 parts of epibromohydrin and 5.8 - 7.2 parts of DBU, stir and react at 25 - 35 °C for 2 - 4 h to obtain a crude product, remove the excess acetone, and then dilute and wash the crude product to obtain the bio-based epoxy resin.

[0021] Preferably, the preparation method of the bio-based epoxy curing agent comprises the following steps:

[0022] Mix 10 - 20 parts of cardanol, 3 - 7 parts of triethylamine, and 14 - 20 parts of chloroform evenly by stirring, then dropwise add 9 - 18 parts of diphenyl chlorophosphate, carry out condensation reflux at 60 - 70 °C for 4 - 7 h, after the reaction, filter to remove the solid precipitate, wash the obtained filtrate multiple times, collect the organic phase and dry it, and remove chloroform to obtain an intermediate product; add the intermediate product to 3.4 - 6.8 parts of diethylenetriamine and mix and stir evenly, then gradually dropwise add 2.7 - 5.4 parts of formaldehyde solution, carry out condensation reflux at 85 - 95 °C for 3 - 5 h, and then heat to 110 - 140 °C to remove water to obtain the bio-based epoxy curing agent.

[0023] Preferably, the preparation method of the modified hollow glass microspheres comprises the following steps:

[0024] Add the alkali-treated hollow glass microbeads to the chitosan acetate solution, mix and stir for 30 - 90 min, then adjust the pH value of the mixed solution to 6 - 10, and continue to stir for 20 - 40 min to obtain the modified hollow glass microbeads.

[0025] In summary, the present application includes at least one of the following beneficial technical effects:

[0026] 1. The present application uses bio-based epoxy resin and bio-based epoxy curing agent as the key components of the grout material, and adds compounded matte silica, hydrophobic fumed silica, and modified hollow glass microspheres, so that the prepared grout has good anti-ultraviolet performance, antibacterial and mildew-proof performance, flame retardant performance, and has a matte texture. The material composition is safe, the VOC emission is low, it is environmentally friendly, green and sustainable, and the bonding strength and strength of the product are high, ensuring a firm bond between the grout and substrates such as tiles and stones, and it is not easy to fall off. Detailed implementation manners

[0027] The present application will be further described in detail below with reference to the embodiments.

[0028] Preparation examples

[0029] Preparation example 1 Preparation of bio-based epoxy resin

[0030] Preparation example 1.1

[0031] Mix 21.6 g of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, 70 g of xylene, and 3 g of a 1% chloroplatinic acid isopropanol solution as a catalyst evenly, heat to 120 °C, then drop in 13 g of itaconic acid, and react for 12 h to obtain an intermediate product; cool the intermediate product to room temperature, then filter to remove the filtrate, wash the solid intermediate product several times with acetone, and vacuum dry it at 95 °C for 4 h. Then add the intermediate product to 60 g of acetone, add 5.2 g of epibromohydrin and 5.8 g of DBU, stir and react at 25 °C for 4 h to obtain a crude product. After removing the excess acetone, dilute the crude product with toluene and wash it five times with deionized water to obtain the bio-based epoxy resin, phosphorus-containing itaconic acid-based epoxy resin.

[0032] Preparation example 1.2

[0033] Mix 32.4 g of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, 105 g of xylene, and 4.5 g of a 1% chloroplatinic acid isopropanol solution as a catalyst evenly, heat to 130 °C, then drop in 19 g of itaconic acid, and react for 16 h to obtain an intermediate product; cool the intermediate product to room temperature, then filter to remove the filtrate, wash the solid intermediate product several times with acetone, and vacuum dry it at 90 °C for 5 h. Then add the intermediate product to 65 g of acetone, add 6 g of epibromohydrin and 6.3 g of DBU, stir and react at 30 °C for 3 h to obtain a crude product. After removing the excess acetone, dilute the crude product with toluene and wash it five times with deionized water to obtain the bio-based epoxy resin, phosphorus-containing itaconic acid-based epoxy resin.

[0034] Preparation Example 1.3

[0035] 43.2 g of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, 140 g of xylene, and 6 g of an isopropyl alcohol solution of chloroplatinic acid with a catalyst concentration of 1% were mixed evenly, heated to 140 °C, and then 26 g of itaconic acid was dropped in. The reaction was carried out for 20 h, and an intermediate product was obtained after the reaction. The intermediate product was cooled to room temperature, then the filtrate was removed by filtration, the solid intermediate product was washed several times with acetone, and after vacuum drying at 85 °C for 6 h, the intermediate product was added to 70 g of acetone, 6.8 g of epibromohydrin and 7.2 g of DBU were added, and the reaction was stirred at 35 °C for 2 h to obtain a crude product. After removing the excess acetone, the crude product was diluted with toluene and washed five times with deionized water to obtain a bio-based epoxy resin containing phosphorus itaconic acid-based epoxy resin.

[0036] Preparation Example 2 Preparation of Bio-based Epoxy Curing Agent

[0037] Preparation Example 2.1

[0038] 10 g of cardanol, 3 g of triethylamine, and 14 g of chloroform were mixed and stirred evenly, then 9 g of diphenyl chlorophosphate was dropped in, and the reaction was carried out under reflux condensation at 60 °C for 7 h. After the reaction, the solid precipitate was removed by suction filtration, the obtained filtrate was washed several times, the organic phase was collected and dried with anhydrous sodium sulfate, and the chloroform was removed by rotary evaporation to obtain an intermediate product. The intermediate product was added to 3.4 g of diethylenetriamine and mixed and stirred evenly, and then 2.7 g of a 37% formaldehyde solution by mass was added dropwise. After reflux condensation at 85 °C for 5 h, the temperature was raised to 110 °C to remove water, and a bio-based epoxy curing agent containing phosphorus cardanol-based curing agent was obtained.

[0039] Preparation Example 2.2

[0040] 15 g of cardanol, 5 g of triethylamine, and 17 g of chloroform were mixed and stirred evenly, then 13.5 g of diphenyl chlorophosphate was dropped in, and the reaction was carried out under reflux condensation at 65 °C for 6 h. After the reaction, the solid precipitate was removed by suction filtration, the obtained filtrate was washed several times, the organic phase was collected and dried with anhydrous sodium sulfate, and the chloroform was removed by rotary evaporation to obtain an intermediate product. The intermediate product was added to 5.1 g of diethylenetriamine and mixed and stirred evenly, and then 4 g of a 37% formaldehyde solution by mass was added dropwise. After reflux condensation at 90 °C for 4 h, the temperature was raised to 125 °C to remove water, and a bio-based epoxy curing agent containing phosphorus cardanol-based curing agent was obtained.

[0041] Preparation Example 2.3

[0042] After mixing 20 g of cardanol, 7 g of triethylamine, and 20 g of chloroform and stirring them evenly, 18 g of diphenyl chlorophosphate was dropped in, and the mixture was refluxed under condensation at 70 °C for 4 h. After the reaction was completed, the solid precipitate was removed by suction filtration. The obtained filtrate was washed several times, the organic phase was collected and dried with anhydrous sodium sulfate, and chloroform was removed by rotary evaporation to obtain an intermediate product; the intermediate product was added to 6.8 g of diethylenetriamine and stirred evenly, and then 5.4 g of a 37% formaldehyde solution by mass was added dropwise. After refluxing under condensation at 95 °C for 3 h, the temperature was raised to 140 °C to remove water, and a bio-based epoxy curing agent containing phosphorus cardanol-based curing agent was obtained.

[0043] Preparation Example 3 Preparation of Modified Hollow Glass Microspheres

[0044] Preparation Example 3.1

[0045] S1. Add 5 g of hollow glass microspheres to 40 g of a 30% sodium hydroxide solution by mass, stir for 1 h, filter to remove the filtrate, and wash the solid several times with deionized water to obtain alkali-treated hollow glass microspheres;

[0046] S2. Add low-viscosity chitosan to an acetic acid solution and stir evenly to prepare a chitosan acetic acid solution with a concentration of 5 g / L;

[0047] S3. Add the alkali-treated hollow glass microspheres to the chitosan acetic acid solution at a solid-liquid ratio of 1:8 g / mL, mix and stir for 30 min, then adjust the pH value of the mixed solution to 6, and continue to stir for 20 min to cure the chitosan molecules adsorbed on the surface of the hollow glass microspheres to form a dense chitosan deposition film, obtaining modified hollow glass microspheres.

[0048] Preparation Example 3.2

[0049] S1. Add 10 g of hollow glass microspheres to 60 g of a 30% sodium hydroxide solution by mass, stir for 1.5 h, filter to remove the filtrate, and wash the solid several times with deionized water to obtain alkali-treated hollow glass microspheres;

[0050] S2. Add low-viscosity chitosan to an acetic acid solution and stir evenly to prepare a chitosan acetic acid solution with a concentration of 3 g / L;

[0051] S3. Add the alkali-treated hollow glass microspheres to the chitosan acetic acid solution at a solid-liquid ratio of 1:11 g / mL, mix and stir for 60 min, then adjust the pH value of the mixed solution to 8, and continue to stir for 30 min to cure the chitosan molecules adsorbed on the surface of the hollow glass microspheres to form a dense chitosan deposition film, obtaining modified hollow glass microspheres.

[0052] Preparation Example 3.3

[0053] S1. Add 15 g of hollow glass microspheres to 80 g of a 30% sodium hydroxide solution by mass, stir for 2 h, filter to remove the filtrate, and wash the solid with deionized water several times to obtain alkali-treated hollow glass microspheres;

[0054] S2. Add low-viscosity chitosan to an acetic acid solution and stir evenly to prepare a chitosan acetic acid solution with a concentration of 1 g / L;

[0055] S3. Add the alkali-treated hollow glass microspheres to the chitosan acetic acid solution at a solid-liquid ratio of 1:14 g / mL, mix and stir for 90 min, then adjust the pH value of the mixture to 10 and continue stirring for 40 min to solidify the chitosan molecules adsorbed on the surface of the hollow glass microspheres, forming a dense chitosan deposition film to obtain modified hollow glass microspheres.

[0056] Example

[0057] Example 1

[0058] Mix 75 g of the bio-based epoxy resin prepared in Preparation Example 1.1, 1 g of BYK-2155 dispersant, 1 g of Disperbyk-900 defoamer, 8 g of compounded matting silica, 10 g of hydrophobic fumed silica, and 5 g of the modified hollow glass microspheres prepared in Preparation Example 3.1 evenly to obtain the Component A;

[0059] Mix 70 g of the bio-based epoxy curing agent prepared in Preparation Example 3.1, 5 g of hydrophobic fumed silica, 8 g of compounded matting silica, 5 g of the modified hollow glass microspheres prepared in Preparation Example 3.1, and 5 g of color paste evenly to obtain the Component B; in this example, the compounded matting silica raw material includes 10% Tosoh SS20 matting silica, 15% Grace ED60 matting silica, 10% Evonik TS100 matting silica, and 65% Aerospace Saide 690 matting silica by mass percentage.

[0060] Example 2

[0061] Mix 75 g of the bio-based epoxy resin prepared in Preparation Example 1.1, 1.25 g of BYK-2155 dispersant, 1.25 g of Disperbyk-900 defoamer, 9 g of compounded matting silica, 11 g of hydrophobic fumed silica, and 5 g of the modified hollow glass microspheres prepared in Preparation Example 3.1 evenly to obtain the Component A;

[0062] 70 g of the bio-based epoxy curing agent prepared in Preparation Example 3.1, 6.5 g of hydrophobic fumed silica, 9 g of compounded matting silica, 5 g of modified hollow glass microspheres prepared in Preparation Example 3.1, and 6 g of color paste were mixed evenly to obtain the B component; the compounded matting silica raw material used in this example included 15% Tosoh SS20 matting silica, 20% Grace ED60 matting silica, 15% Evonik TS100 matting silica, and 50% Aerospace Saide 690 matting silica by mass percentage.

[0063] Example 3

[0064] 75 g of the bio-based epoxy resin prepared in Preparation Example 1.1, 1.5 g of BYK-2155 dispersant, 1.5 g of Disperbyk 900 defoamer, 10 g of compounded matting silica, 12 g of hydrophobic fumed silica, and 5 g of modified hollow glass microspheres prepared in Preparation Example 3.1 were mixed evenly to obtain the A component;

[0065] 70 g of the bio-based epoxy curing agent prepared in Preparation Example 3.1, 8 g of hydrophobic fumed silica, 10 g of compounded matting silica, 5 g of modified hollow glass microspheres prepared in Preparation Example 3.1, and 7 g of color paste were mixed evenly to obtain the B component; the compounded matting silica raw material used in this example included 20% Tosoh SS20 matting silica, 25% Grace ED60 matting silica, 20% Evonik TS100 matting silica, and 35% Aerospace Saide 690 matting silica by mass percentage.

[0066] Example 4

[0067] The difference between Example 4 and Example 1 was that the bio-based epoxy resin used in Example 4 was from Preparation Example 1.1 and had a mass of 80 g.

[0068] Example 5

[0069] The difference between Example 5 and Example 1 was that the bio-based epoxy resin used in Example 5 was from Preparation Example 1.1 and had a mass of 85 g.

[0070] Example 6

[0071] The difference between Example 6 and Example 1 was that the bio-based epoxy resin used in Example 6 was from Preparation Example 1.2 and had a mass of 75 g.

[0072] Example 7

[0073] The difference between Example 7 and Example 1 was that the bio-based epoxy resin used in Example 7 was from Preparation Example 1.3 and had a mass of 75 g.

[0074] Example 8

[0075] Example 8 is different from Example 1 in that the bio-based epoxy curing agent used in Example 8 is from Preparation Example 2.1 and has a mass of 75 g.

[0076] Example 9

[0077] Example 9 is different from Example 1 in that the bio-based epoxy curing agent used in Example 9 is from Preparation Example 2.1 and has a mass of 80 g.

[0078] Example 10

[0079] Example 10 is different from Example 1 in that the bio-based epoxy curing agent used in Example 10 is from Preparation Example 2.2 and has a mass of 70 g.

[0080] Example 11

[0081] Example 11 is different from Example 1 in that the bio-based epoxy curing agent used in Example 11 is from Preparation Example 2.3 and has a mass of 70 g.

[0082] Example 12

[0083] Example 12 is different from Example 1 in that the modified hollow glass microspheres used in Component A and Component B of Example 12 are both from Preparation Example 3.1 and have a mass of 7.5 g each.

[0084] Example 13

[0085] Example 13 is different from Example 1 in that the modified hollow glass microspheres used in Component A and Component B of Example 13 are both from Preparation Example 3.1 and have a mass of 10 g each.

[0086] Example 14

[0087] Example 14 is different from Example 1 in that the modified hollow glass microspheres used in Component A and Component B of Example 14 are both from Preparation Example 3.2 and have a mass of 5 g each.

[0088] Example 15

[0089] Example 15 is different from Example 1 in that the modified hollow glass microspheres used in Component A and Component B of Example 15 are both from Preparation Example 3.3 and have a mass of 5 g each.

[0090] Comparative Example

[0091] Comparative Example 1

[0092] Comparative Example 1 is different from Example 1 in that the bio-based epoxy resin used in Comparative Example 1 is from Preparation Example 1.1 and has a mass of 65 g.

[0093] Comparative Example 2

[0094] The difference between Comparative Example 2 and Example 1 is that the bio-based epoxy resin used in Comparative Example 2 is from Preparation Example 1.1 and has a mass of 95 g.

[0095] Comparative Example 3

[0096] The difference between Comparative Example 3 and Example 1 is that the bio-based epoxy curing agent used in Comparative Example 3 is from Preparation Example 2.1 and has a mass of 60 g.

[0097] Comparative Example 4

[0098] The difference between Comparative Example 4 and Example 1 is that the bio-based epoxy curing agent used in Comparative Example 4 is from Preparation Example 2.1 and has a mass of 90 g.

[0099] Comparative Example 5

[0100] The difference between Comparative Example 5 and Example 1 is that the modified hollow glass microspheres used in Component A and Component B in Comparative Example 5 are both from Preparation Example 3.1 and each has a mass of 2 g.

[0101] Comparative Example 6

[0102] The difference between Comparative Example 6 and Example 1 is that the modified hollow glass microspheres used in Component A and Component B in Comparative Example 6 are both from Preparation Example 3.1 and each has a mass of 13 g.

[0103] Comparative Example 7

[0104] The difference between Comparative Example 7 and Example 1 is that the hollow glass microspheres used in Component A and Component B in Comparative Example 7 are both unmodified hollow glass microspheres and each has a mass of 5 g.

[0105] Performance Detection Test

[0106] 1. The caulking agents of Examples 1 - 15 and Comparative Examples 1 - 7 were respectively mixed according to the volume ratio of Component A to Component B of 1:1, and then the appearance texture, bond strength, and surface drying time were tested according to the standard of Q / SY YHF 0099 - 2021;

[0107] 2. The glossiness was tested using a glossiness meter from Shenzhen 3nh Technology Co., Ltd. according to the standard of T / CBMF 166—2022;

[0108] 3. The color difference was tested using an array spectrophotometric colorimeter from Shenzhen 3nh Technology Co., Ltd. according to the standard of T / CBMF 166—2022; 4. The antibacterial rate was tested according to GB / T 1741 - 2007 "Determination Method for Resistance of Paint Films to Mildew";

[0109] 5. Conduct a vertical burning test in accordance with the FMVSS 302 / ZSO 3975 standard;

[0110] The results are shown in Table 1.

[0111] The specific test results are as follows:

[0112] Table 1 Performance Test Results

[0113]

[0114]

[0115]

[0116] It can be seen from the test results in Table 1 that a bio-based epoxy matte joint sealant and its preparation method provided by the present application can obtain a bio-based joint sealant with remarkable dullness, UV resistance, bonding strength, surface drying time, flame retardancy and antibacterial rate, and the components of the bio-based joint sealant are more green, low-carbon and environmentally friendly, and have less impact on the environment.

[0117] This specific embodiment is only an explanation of the present application and does not limit the present application. After reading this specification, those skilled in the art can make modifications to this embodiment without creative contributions as needed, but as long as they are within the scope of the claims of the present application, they are protected by the patent law.

Claims

1. A bio-based epoxy matte seam beautifying agent, characterized in that: The seam beautifying agent includes component A and component B; In parts by mass, the component A includes: 75-85 parts of bio-based epoxy resin, 1-1.5 parts of dispersant, 1-1.5 parts of defoamer, 8-10 parts of compound matte silica, 10-12 parts of hydrophobic fumed silica, and 5-10 parts of modified hollow glass microspheres; In terms of mass fraction, the component B comprises: 70-80 parts of a bio-based epoxy curing agent, 5-8 parts of hydrophobic fumed silica, 8-10 parts of compounded matte silica, 5-10 parts of modified hollow glass microspheres, and 5-7 parts of a color paste; The bio-based epoxy resin is a phosphorus-containing itaconic acid-based epoxy resin; the phosphorus-containing itaconic acid-based epoxy resin is prepared from the following raw materials in parts by weight: 21.6-43.2 parts of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, 70-140 parts of xylene, 3-6 parts of catalyst, 13-26 parts of itaconic acid, 60-70 parts of acetone, 5.2-6.8 parts of epibromopropane, and 5.8-7.2 parts of DBU; The bio-based epoxy curing agent is a phosphorus-containing cardanol-based curing agent; the phosphorus-containing cardanol-based curing agent is prepared from the following raw materials in parts by weight: 10-20 parts of cardanol, 3-7 parts of triethylamine, 14-20 parts of chloroform, 9-18 parts of diphenyl chlorophosphate, 3.4-6.8 parts of diethylenetriamine, and 2.7-5.4 parts of formaldehyde solution; The modified hollow glass microsphere raw material includes alkali-treated hollow glass microspheres and chitosan acetic acid solution with a concentration of 1-5 g / L, and the solid-liquid ratio of the two is 1:8-14 g / mL; The preparation method of the modified hollow glass microspheres comprises the following steps: adding alkali-treated hollow glass microspheres into chitosan acetic acid solution, mixing and stirring for 30-90 minutes, adjusting the pH value of the mixed solution to 6-10, and continuing stirring for 20-40 minutes to obtain the modified hollow glass microspheres.

2. The bio-based epoxy matte seam beautifying agent according to claim 1, characterized in that: The dispersant is BYK-2155 type dispersant.

3. The bio-based epoxy matte seam beautifying agent according to claim 1, characterized in that: The defoamer is Digo 900 type defoamer.

4. A method for preparing a bio-based epoxy matte seam beautifying agent according to any one of claims 1 to 3, characterized in that: The following steps are involved: 75-85 parts of bio-based epoxy resin, 1-1.5 parts of dispersant, 1-1.5 parts of defoamer, 8-10 parts of compound matte silica, 10-12 parts of hydrophobic fumed silica, and 5-10 parts of modified hollow glass microspheres are mixed uniformly by weight to obtain the component A; 70-80 parts of bio-based epoxy curing agent, 5-8 parts of hydrophobic fumed silica, 8-10 parts of compound matte silica, 5-10 parts of modified hollow glass microspheres, and 5-7 parts of color paste are mixed uniformly by weight to obtain the B component.

5. The method for preparing a bio-based epoxy matte seam beautifying agent according to claim 4, characterized in that: The preparation method of the bio-based epoxy resin comprises the following steps: 21.6-43.2 parts of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, 70-140 parts of xylene and 3-6 parts of catalyst are uniformly mixed, heated to 120-140°C, then 13-26 parts of itaconic acid are dropped, and the reaction is carried out for 12-20 hours. After the reaction is completed, an intermediate product is obtained; the intermediate product is cooled to room temperature, then filtered, washed and vacuum dried for 4-6 hours, and then the intermediate product is added to 60-70 parts of acetone, 5.2-6.8 parts of epibromopropane and 5.8-7.2 parts of DBU are added, and the reaction is stirred at 25-35°C for 2-4 hours to obtain a crude product. After removing excess acetone, the crude product is diluted and washed to obtain a bio-based epoxy resin.

6. The method for preparing a bio-based epoxy matte seam beautifying agent according to claim 4, characterized in that: The preparation method of the bio-based epoxy curing agent comprises the following steps: 10-20 parts of cardanol, 3-7 parts of triethylamine and 14-20 parts of chloroform are mixed and stirred evenly, and then 9-18 parts of diphenyl chlorophosphate are added dropwise, and the mixture is condensed and refluxed at 60-70°C for 4-7 hours. After the reaction is completed, the solid precipitate is removed by suction filtration, and the obtained filtrate is washed for multiple times. The organic phase is collected and dried, and the chloroform is removed to obtain an intermediate product; the intermediate product is added to 3.4-6.8 parts of diethylenetriamine, mixed and stirred evenly, and then 2.7-5.4 parts of formaldehyde solution are added dropwise, and the mixture is condensed and refluxed at 85-95°C for 3-5 hours, and then the temperature is raised to 110-140°C to remove water to obtain a bio-based epoxy curing agent.

7. The method for preparing a bio-based epoxy matte seam beautifying agent according to claim 4, characterized in that: The method for preparing the modified hollow glass microspheres comprises the following steps: The alkali-treated hollow glass microspheres are added to the chitosan acetic acid solution, mixed and stirred for 30-90 minutes, the pH value of the mixed solution is adjusted to 6-10, and the stirring is continued for 20-40 minutes to obtain modified hollow glass microspheres.

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