A colored sand self-leveling floor paint and a preparation method thereof
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2024-11-15
- Publication Date
- 2026-08-11
AI Technical Summary
[0003]本发明的目的在于提供一种彩砂自流平地坪涂料及其制备方法,解决了现阶段彩砂自流平地坪涂料长时间使用会出现明显磨损,且被水浸泡后会出现桥边的问题
[0020]在组分A和组分B共混后由于改性填料表面含有环氧基,固化促进剂上含有氨基,二者能够参与到环氧树脂分子固化中,强化填料的加入能够增加分子交联密度,进而提升了材料的耐磨效果,同时以纤维素作为强化填料的基材,能够增加涂料的裂纹扩展阻力,延迟裂纹的扩展,并在裂纹尖端形成纤维桥接,从而提高涂料的断裂韧性,同时表面包覆含有有机硅的链段的共聚物,能够增加改性填料的疏水效果,且与固化促进剂上的长链烷基配合,增加了涂料的耐水性,长链烷基能够与环氧树脂分子之间的界面可以形成一个过渡层,这个过渡层可以增加材料内部的裂纹扩展阻力,从而提高涂料的韧性。
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Abstract
Description
Technical Field
[0001] This invention relates to the field of colored sand self-leveling preparation technology, specifically to a colored sand self-leveling floor coating and its preparation method. Background Technology
[0002] Epoxy resin is widely used in the decoration and renovation of building floors, thanks to the rapid development of solvent-free liquid epoxy resin and the improvement of construction technology and equipment. Currently, epoxy resin flooring products are comprehensive, including solvent-based epoxy wear-resistant floor coatings, water-based epoxy floor coatings, outdoor weather-resistant floor coatings, epoxy self-leveling floor coatings, and anti-static epoxy floor coatings. Epoxy colored sand self-leveling flooring is a seamless, integrated new type of composite decorative flooring composed of colored quartz sand and special epoxy resin. It allows for the free combination of one or more different colored quartz sands to create a variety of decorative patterns. The colored sand used in epoxy colored sand self-leveling flooring is generally natural colored sand, such as natural colored marble and granite sand particles. It has natural colors, never changes color, has good compressive strength, and the construction effect is close to that of natural stone. However, because epoxy resin is relatively brittle after curing, the self-leveling flooring is prone to damage or wear during use. Furthermore, bridging can occur after soaking in water, affecting normal use. Summary of the Invention
[0003] The purpose of this invention is to provide a colored sand self-leveling floor coating and its preparation method, which solves the problems of obvious wear and tear after long-term use of colored sand self-leveling floor coatings and the appearance of bridge edges after being soaked in water.
[0004] The objective of this invention can be achieved through the following technical solutions:
[0005] A method for preparing a colored sand self-leveling floor coating specifically includes the following steps:
[0006] Step A1: Cashew nut phenol, potassium carbonate, allyl chloride and toluene are mixed evenly and reacted at a speed of 150-200 r / min and a temperature of 20-25℃ for 3-5 h to obtain intermediate 1. Intermediate 1, tetramethylcyclotetrasiloxane, chloroplatinic acid and DMF are mixed evenly and reacted under nitrogen protection at a speed of 120-150 r / min and a temperature of 70-80℃ for 3-5 h to obtain intermediate 2.
[0007] Step A2: Mix intermediate 2, octamethylcyclotetrasiloxane, tetramethylammonium hydroxide, 1,3-bis(3-aminopropyl)-1,1,3,3-tetramethyldisiloxane and dimethyl sulfoxide evenly, purge with nitrogen, and react for 3-5 hours at a speed of 120-150 r / min and a temperature of 105-110℃ to obtain a curing accelerator. Disperse the modified filler in ethanol, and stir and add KH560 and deionized water at a speed of 200-300 r / min and a temperature of 25-30℃ to obtain a reinforced filler.
[0008] Step A3: Weigh the following raw materials by weight: 80-90 parts epoxy resin E-51, 10-20 parts reinforcing filler and 10-20 parts 501A epoxy reactive diluent, mix them evenly to obtain component A. Weigh the following raw materials by weight: 15-20 parts curing agent, 5-10 parts curing accelerator, 100-150 parts colored sand, 2-5 parts talc powder, 0.3-1 part dispersant, 0.3-0.5 parts defoamer and 5-10 parts leveling agent, mix them evenly to obtain component B. Mix component A and component B to obtain colored sand self-leveling floor coating.
[0009] Furthermore, in step A1, the molar ratio of cashew phenol, potassium carbonate, and allyl chloride is 1:1.1:1, the molar ratio of intermediate 1 and tetramethylcyclotetrasiloxane is 1:4, and the amount of chloroplatinic acid used is 1‰ of the mass of tetramethylcyclotetrasiloxane.
[0010] Furthermore, the molar ratio of intermediate 2, octamethylcyclotetrasiloxane, tetramethylammonium hydroxide and 1,3-bis(3-aminopropyl)-1,1,3,3-tetramethyldisiloxane described in step A2 is 1.2:1.2:3:2, and the amount of KH560 used is 5% of the mass of the modified filler.
[0011] Furthermore, the modified filler is prepared by the following steps:
[0012] Step B1: Disperse cellulose in N,N-dimethylacetamide, purge with nitrogen, and stir at 120-150 r / min and 100-110℃ while adding anhydrous lithium chloride. Stir for 3-5 h, cool to 8-10℃, add triethylamine and p-toluenesulfonyl chloride, and react for 20-25 h to obtain pretreated cellulose. Disperse the pretreated cellulose in N,N-dimethylacetamide, and stir at 60-80 r / min and 140-145℃ while adding ammonia. React for 20-25 h to obtain aminated cellulose.
[0013] Step B2: Aminated cellulose, maleic anhydride, triethylamine, and N,N-dimethylformamide are mixed evenly and reacted at 120-150 r / min and 80-90℃ for 6-8 h to obtain modified cellulose. Tetramethyltri-3-trifluoropropylcyclotetrasiloxane, octamethylcyclotetrasiloxane, tetramethylammonium hydroxide, 1,3-bis(3-aminopropyl)-1,1,3,3-tetramethyldisiloxane, and dimethyl sulfoxide are mixed evenly and reacted under nitrogen protection at 120-150 r / min and 105-110℃ for 3-5 h to obtain the modifier.
[0014] Step B3: Mix the modifier, allyl glycidyl ether, and N,N-dimethylformamide evenly, and react them for 6-8 hours at a speed of 150-200 r / min, a temperature of 60-70℃, and a pH of 9-10 to obtain the modified monomer. Mix the modified monomer, modified cellulose, 1-hexene, azobisisobutyronitrile, and N,N-dimethylformamide evenly, and purge with nitrogen gas. React them for 10-12 hours at a speed of 120-150 r / min and a temperature of 70-75℃ to obtain the modified filler.
[0015] Furthermore, in step B1, the mass ratio of cellulose, anhydrous lithium chloride, triethylamine, and p-toluenesulfonyl chloride is 10 mg: 1 mg: 1 g: 5 g, and the volume ratio of pretreated cellulose, N,N-dimethylacetamide, and ammonia is 1 mL: 10 mL: 20 mL, with the ammonia having a mass fraction of 30%.
[0016] Furthermore, in step B2, the molar ratio of amino groups, maleic anhydride, and triethylamine on the aminated cellulose is 1:1:1.2, and the molar ratio of tetramethyltri-3-trifluoropropylcyclotetrasiloxane, octamethylcyclotetrasiloxane, tetramethylammonium hydroxide, and 1,3-bis(3-aminopropyl)-1,1,3,3-tetramethyldisiloxane is 1.5:0.9:3:2.
[0017] Furthermore, the molar ratio of the modifier and allyl glycidyl ether mentioned in step B3 is 1:4, the molar ratio of the modified monomer, modified cellulose and 1-hexene is 60 mmol:1 g:40 mmol, and the amount of azobisisobutyronitrile is 1% of the mass of 1-hexene.
[0018] The beneficial effects of the present invention: The colored sand self-leveling floor coating prepared by the present invention includes component A and component B. Component A includes the following raw materials: epoxy resin E-51, reinforcing filler and 501A epoxy reactive diluent. Component B includes the following raw materials: curing agent, curing accelerator, colored sand, talc powder, dispersant, defoamer and leveling agent. The curing accelerator is made from cashew phenol and allyl chloride. Under the action of potassium carbonate, the hydroxyl groups on cashew phenol and the chlorine atoms on allyl chloride react to obtain intermediate 1. Intermediate 1 is reacted with tetramethylcyclotetrasiloxane, so that the double bond on intermediate 1 reacts with the SiH bond on tetramethylcyclotetrasiloxane to obtain intermediate 2. Intermediate 2 and octamethylcyclotetrasiloxane are ring-opened, and then polymerized with 1,3-bis(3-aminopropyl)-1,1,3,3-tetramethyldisiloxane to obtain the curing accelerator.
[0019] The reinforcing filler is made from cellulose and treated with p-toluenesulfonyl chloride, causing the hydroxyl groups on the cellulose to react with the acyl chloride on the p-toluenesulfonyl chloride, thus obtaining pretreated cellulose. The pretreated cellulose is then treated with ammonia water, causing the p-benzenesulfonate on the pretreated cellulose to undergo ammonolysis, yielding aminated cellulose. The aminated cellulose is then reacted with maleic anhydride, causing the amino groups on the aminated cellulose to react with the maleic anhydride to form a maleimide structure. The tetramethyltri-3-trifluoropropylcyclotetrasiloxane and octamethylcyclotetrasiloxane are ring-opened, and then reacted with 1,3-bis(3-aminopropyl) A modifier is prepared by polymerizing 1,1,3,3-tetramethyldisiloxane. The modifier is then reacted with allyl glycidyl ether, causing the amino groups on the modifier to react with the epoxy groups on the allyl glycidyl ether, thus preparing a modifying monomer. The modifying monomer, modified cellulose, and 1-hexene are copolymerized in the presence of azobisisobutyronitrile. A copolymer containing organosilicon segments is coated on the surface of the modified cellulose to obtain a modified filler. The modified filler is then treated with KH560, causing the siloxane bonds on KH560 to hydrolyze and graft onto the hydroxyl groups on the modified filler, thus obtaining a reinforcing filler.
[0020] After blending components A and B, the modified filler contains epoxy groups on its surface, and the curing accelerator contains amino groups. Both can participate in the curing of epoxy resin molecules. The addition of reinforcing filler can increase the molecular crosslinking density, thereby improving the wear resistance of the material. At the same time, using cellulose as the base material for reinforcing filler can increase the crack propagation resistance of the coating, delay crack propagation, and form fiber bridging at the crack tip, thereby improving the fracture toughness of the coating. Meanwhile, the copolymer containing organosilicon segments coated on the surface can increase the hydrophobic effect of the modified filler, and in combination with the long-chain alkyl groups on the curing accelerator, it can increase the water resistance of the coating. The long-chain alkyl groups can form a transition layer at the interface between epoxy resin molecules. This transition layer can increase the crack propagation resistance inside the material, thereby improving the toughness of the coating. Detailed Implementation
[0021] The technical solutions in the embodiments of the present invention will be clearly and completely described below. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.
[0022] Example 1: A method for preparing a colored sand self-leveling floor coating, specifically including the following steps:
[0023] Step A1: Cashew phenol, potassium carbonate, allyl chloride and toluene are mixed evenly and reacted at 150 r / min and 20°C for 3 h to obtain intermediate 1. Intermediate 1, tetramethylcyclotetrasiloxane, chloroplatinic acid and DMF are mixed evenly and reacted under nitrogen protection at 120 r / min and 70°C for 3 h to obtain intermediate 2.
[0024] Step A2: Intermediate 2, octamethylcyclotetrasiloxane, tetramethylammonium hydroxide, 1,3-bis(3-aminopropyl)-1,1,3,3-tetramethyldisiloxane and dimethyl sulfoxide are mixed evenly, and nitrogen gas is introduced for protection. The mixture is reacted for 3 hours at a speed of 120 r / min and a temperature of 105℃ to obtain a curing accelerator. The modified filler is dispersed in ethanol, and KH560 and deionized water are added at a speed of 200 r / min and a temperature of 25℃. The mixture is stirred and reacted for 2 hours to obtain a reinforced filler.
[0025] Step A3: Weigh the following raw materials by weight: 80 parts epoxy resin E-51, 10 parts reinforcing filler and 10 parts 501A epoxy reactive diluent, mix them evenly to obtain component A. Weigh the following raw materials by weight: 15 parts curing agent, 5 parts curing accelerator, 100 parts colored sand, 2 parts talc powder, 0.3 parts dispersant, 0.3 parts defoamer and 5 parts leveling agent, mix them evenly to obtain component B. Mix component A and component B to obtain colored sand self-leveling floor coating.
[0026] In step A1, the molar ratio of cashew phenol, potassium carbonate, and allyl chloride is 1:1.1:1, the molar ratio of intermediate 1 and tetramethylcyclotetrasiloxane is 1:4, and the amount of chloroplatinic acid used is 1‰ of the mass of tetramethylcyclotetrasiloxane.
[0027] The molar ratio of intermediate 2, octamethylcyclotetrasiloxane, tetramethylammonium hydroxide and 1,3-bis(3-aminopropyl)-1,1,3,3-tetramethyldisiloxane described in step A2 is 1.2:1.2:3:2, and the amount of KH560 used is 5% of the mass of the modified filler.
[0028] The curing agent mentioned in step A3 is ethylenediamine, the dispersant is BYK-142, the defoamer is BYK-066N, and the leveling agent is BYK-302.
[0029] The modified filler is prepared by the following steps:
[0030] Step B1: Disperse cellulose in N,N-dimethylacetamide, purge with nitrogen, stir and add anhydrous lithium chloride at 120 r / min and 100 °C, stir for 3 h, cool to 8 °C, add triethylamine and p-toluenesulfonyl chloride, react for 20 h to obtain pretreated cellulose. Disperse the pretreated cellulose in N,N-dimethylacetamide, stir and add ammonia at 60 r / min and 140 °C, react for 20 h to obtain aminated cellulose.
[0031] Step B2: Aminated cellulose, maleic anhydride, triethylamine, and N,N-dimethylformamide are mixed evenly and reacted at 120 r / min and 80 °C for 6 h to obtain modified cellulose. Tetramethyltri-3-trifluoropropylcyclotetrasiloxane, octamethylcyclotetrasiloxane, tetramethylammonium hydroxide, 1,3-bis(3-aminopropyl)-1,1,3,3-tetramethyldisiloxane, and dimethyl sulfoxide are mixed evenly and reacted under nitrogen protection at 120 r / min and 105 °C for 3 h to obtain the modifier.
[0032] Step B3: Mix the modifier, allyl glycidyl ether, and N,N-dimethylformamide evenly, and react for 6 hours at a speed of 150 r / min, a temperature of 60℃, and a pH of 9 to obtain the modified monomer. Mix the modified monomer, modified cellulose, 1-hexene, azobisisobutyronitrile, and N,N-dimethylformamide evenly, and purge with nitrogen gas for protection. React for 10 hours at a speed of 120 r / min and a temperature of 70℃ to obtain the modified filler.
[0033] In step B1, the mass ratio of cellulose, anhydrous lithium chloride, triethylamine, and p-toluenesulfonyl chloride is 10 mg: 1 mg: 1 g: 5 g, and the volume ratio of pretreated cellulose, N,N-dimethylacetamide, and ammonia is 1 mL: 10 mL: 20 mL, with the ammonia having a mass fraction of 30%.
[0034] The molar ratio of amino groups, maleic anhydride, and triethylamine on the aminated cellulose described in step B2 is 1:1:1.2, and the molar ratio of tetramethyltri-3-trifluoropropylcyclotetrasiloxane, octamethylcyclotetrasiloxane, tetramethylammonium hydroxide, and 1,3-bis(3-aminopropyl)-1,1,3,3-tetramethyldisiloxane is 1.5:0.9:3:2.
[0035] The molar ratio of the modifier and allyl glycidyl ether mentioned in step B3 is 1:4, the ratio of the modified monomer, modified cellulose and 1-hexene is 60 mmol:1 g:40 mmol, and the amount of azobisisobutyronitrile is 1% of the mass of 1-hexene.
[0036] Example 2: A method for preparing a colored sand self-leveling floor coating, specifically including the following steps:
[0037] Step A1: Cashew phenol, potassium carbonate, allyl chloride and toluene are mixed evenly and reacted at 150 r / min and 25°C for 4 h to obtain intermediate 1. Intermediate 1, tetramethylcyclotetrasiloxane, chloroplatinic acid and DMF are mixed evenly and reacted under nitrogen protection at 120 r / min and 75°C for 4 h to obtain intermediate 2.
[0038] Step A2: Intermediate 2, octamethylcyclotetrasiloxane, tetramethylammonium hydroxide, 1,3-bis(3-aminopropyl)-1,1,3,3-tetramethyldisiloxane and dimethyl sulfoxide are mixed evenly, and nitrogen gas is introduced for protection. The mixture is reacted for 4 hours at a speed of 120 r / min and a temperature of 110 °C to obtain a curing accelerator. The modified filler is dispersed in ethanol, and KH560 and deionized water are added at a speed of 200 r / min and a temperature of 30 °C. The mixture is stirred and reacted for 2 hours to obtain a reinforced filler.
[0039] Step A3: Weigh the following raw materials by weight: 85 parts epoxy resin E-51, 15 parts reinforcing filler and 15 parts 501A epoxy reactive diluent, mix them evenly to obtain component A. Weigh the following raw materials by weight: 18 parts curing agent, 8 parts curing accelerator, 125 parts colored sand, 3.5 parts talc powder, 0.6 parts dispersant, 0.4 parts defoamer and 8 parts leveling agent, mix them evenly to obtain component B. Mix component A and component B to obtain colored sand self-leveling floor coating.
[0040] In step A1, the molar ratio of cashew phenol, potassium carbonate, and allyl chloride is 1:1.1:1, the molar ratio of intermediate 1 and tetramethylcyclotetrasiloxane is 1:4, and the amount of chloroplatinic acid used is 1‰ of the mass of tetramethylcyclotetrasiloxane.
[0041] The molar ratio of intermediate 2, octamethylcyclotetrasiloxane, tetramethylammonium hydroxide and 1,3-bis(3-aminopropyl)-1,1,3,3-tetramethyldisiloxane described in step A2 is 1.2:1.2:3:2, and the amount of KH560 used is 5% of the mass of the modified filler.
[0042] The curing agent mentioned in step A3 is hexamethylenediamine, the dispersant is BYK-163, the defoamer is BYK-011, and the leveling agent is BYK-320.
[0043] The modified filler is prepared by the following steps:
[0044] Step B1: Disperse cellulose in N,N-dimethylacetamide, purge with nitrogen, stir and add anhydrous lithium chloride at 120 r / min and 105 °C, stir for 4 h, cool to 9 °C, add triethylamine and p-toluenesulfonyl chloride, react for 25 h to obtain pretreated cellulose. Disperse the pretreated cellulose in N,N-dimethylacetamide, stir and add ammonia at 60 r / min and 145 °C, react for 20 h to obtain aminated cellulose.
[0045] Step B2: Aminated cellulose, maleic anhydride, triethylamine, and N,N-dimethylformamide are mixed evenly and reacted at 120 r / min and 85°C for 7 h to obtain modified cellulose. Tetramethyltri-3-trifluoropropylcyclotetrasiloxane, octamethylcyclotetrasiloxane, tetramethylammonium hydroxide, 1,3-bis(3-aminopropyl)-1,1,3,3-tetramethyldisiloxane, and dimethyl sulfoxide are mixed evenly and reacted under nitrogen protection at 120 r / min and 110°C for 4 h to obtain the modifier.
[0046] Step B3: Mix the modifier, allyl glycidyl ether, and N,N-dimethylformamide evenly, and react for 7 hours at a speed of 150 r / min, a temperature of 65℃, and a pH of 9 to obtain the modified monomer. Mix the modified monomer, modified cellulose, 1-hexene, azobisisobutyronitrile, and N,N-dimethylformamide evenly, purge with nitrogen for protection, and react for 10 hours at a speed of 120 r / min and a temperature of 75℃ to obtain the modified filler.
[0047] In step B1, the mass ratio of cellulose, anhydrous lithium chloride, triethylamine, and p-toluenesulfonyl chloride is 10 mg: 1 mg: 1 g: 5 g, and the volume ratio of pretreated cellulose, N,N-dimethylacetamide, and ammonia is 1 mL: 10 mL: 20 mL, with the ammonia having a mass fraction of 30%.
[0048] The molar ratio of amino groups, maleic anhydride, and triethylamine on the aminated cellulose described in step B2 is 1:1:1.2, and the molar ratio of tetramethyltri-3-trifluoropropylcyclotetrasiloxane, octamethylcyclotetrasiloxane, tetramethylammonium hydroxide, and 1,3-bis(3-aminopropyl)-1,1,3,3-tetramethyldisiloxane is 1.5:0.9:3:2.
[0049] The molar ratio of the modifier and allyl glycidyl ether mentioned in step B3 is 1:4, the ratio of the modified monomer, modified cellulose and 1-hexene is 60 mmol:1 g:40 mmol, and the amount of azobisisobutyronitrile is 1% of the mass of 1-hexene.
[0050] Example 3: A method for preparing a colored sand self-leveling floor coating, specifically including the following steps:
[0051] Step A1: Cashew phenol, potassium carbonate, allyl chloride and toluene are mixed evenly and reacted at 200 r / min and 25°C for 5 h to obtain intermediate 1. Intermediate 1, tetramethylcyclotetrasiloxane, chloroplatinic acid and DMF are mixed evenly and reacted under nitrogen protection at 150 r / min and 80°C for 5 h to obtain intermediate 2.
[0052] Step A2: Intermediate 2, octamethylcyclotetrasiloxane, tetramethylammonium hydroxide, 1,3-bis(3-aminopropyl)-1,1,3,3-tetramethyldisiloxane and dimethyl sulfoxide are mixed evenly, and nitrogen gas is introduced for protection. The mixture is reacted for 5 hours at a speed of 150 r / min and a temperature of 110℃ to obtain a curing accelerator. The modified filler is dispersed in ethanol, and KH560 and deionized water are added at a speed of 300 r / min and a temperature of 30℃. The mixture is stirred and reacted for 3 hours to obtain a reinforced filler.
[0053] Step A3: Weigh the following raw materials by weight: 90 parts epoxy resin E-51, 20 parts reinforcing filler and 20 parts 501A epoxy reactive diluent, mix them evenly to obtain component A. Weigh the following raw materials by weight: 20 parts curing agent, 10 parts curing accelerator, 150 parts colored sand, 5 parts talc powder, 1 part dispersant, 0.5 parts defoamer and 10 parts leveling agent, mix them evenly to obtain component B. Mix component A and component B to obtain colored sand self-leveling floor coating.
[0054] In step A1, the molar ratio of cashew phenol, potassium carbonate, and allyl chloride is 1:1.1:1, the molar ratio of intermediate 1 and tetramethylcyclotetrasiloxane is 1:4, and the amount of chloroplatinic acid used is 1‰ of the mass of tetramethylcyclotetrasiloxane.
[0055] The molar ratio of intermediate 2, octamethylcyclotetrasiloxane, tetramethylammonium hydroxide and 1,3-bis(3-aminopropyl)-1,1,3,3-tetramethyldisiloxane described in step A2 is 1.2:1.2:3:2, and the amount of KH560 used is 5% of the mass of the modified filler.
[0056] The curing agent mentioned in step A3 is diethylenetriamine, the dispersant is BYK-190, the defoamer is BYK-028, and the leveling agent is BYK-420.
[0057] The modified filler is prepared by the following steps:
[0058] Step B1: Disperse cellulose in N,N-dimethylacetamide, purge with nitrogen, stir and add anhydrous lithium chloride at 150 r / min and 110 °C, stir for 5 h, cool to 10 °C, add triethylamine and p-toluenesulfonyl chloride, react for 25 h to obtain pretreated cellulose. Disperse the pretreated cellulose in N,N-dimethylacetamide, stir and add ammonia at 80 r / min and 145 °C, react for 25 h to obtain aminated cellulose.
[0059] Step B2: Aminated cellulose, maleic anhydride, triethylamine, and N,N-dimethylformamide are mixed evenly and reacted at 150 r / min and 90 °C for 8 h to obtain modified cellulose. Tetramethyltri-3-trifluoropropylcyclotetrasiloxane, octamethylcyclotetrasiloxane, tetramethylammonium hydroxide, 1,3-bis(3-aminopropyl)-1,1,3,3-tetramethyldisiloxane, and dimethyl sulfoxide are mixed evenly and reacted under nitrogen protection at 150 r / min and 110 °C for 5 h to obtain the modifier.
[0060] Step B3: Mix the modifier, allyl glycidyl ether, and N,N-dimethylformamide evenly, and react for 8 hours at a speed of 200 r / min, a temperature of 70℃, and a pH of 10 to obtain the modified monomer. Mix the modified monomer, modified cellulose, 1-hexene, azobisisobutyronitrile, and N,N-dimethylformamide evenly, and purge with nitrogen gas for protection. React for 12 hours at a speed of 150 r / min and a temperature of 75℃ to obtain the modified filler.
[0061] In step B1, the mass ratio of cellulose, anhydrous lithium chloride, triethylamine, and p-toluenesulfonyl chloride is 10 mg: 1 mg: 1 g: 5 g, and the volume ratio of pretreated cellulose, N,N-dimethylacetamide, and ammonia is 1 mL: 10 mL: 20 mL, with the ammonia having a mass fraction of 30%.
[0062] The molar ratio of amino groups, maleic anhydride, and triethylamine on the aminated cellulose described in step B2 is 1:1:1.2, and the molar ratio of tetramethyltri-3-trifluoropropylcyclotetrasiloxane, octamethylcyclotetrasiloxane, tetramethylammonium hydroxide, and 1,3-bis(3-aminopropyl)-1,1,3,3-tetramethyldisiloxane is 1.5:0.9:3:2.
[0063] The molar ratio of the modifier and allyl glycidyl ether mentioned in step B3 is 1:4, the ratio of the modified monomer, modified cellulose and 1-hexene is 60 mmol:1 g:40 mmol, and the amount of azobisisobutyronitrile is 1% of the mass of 1-hexene.
[0064] Comparative Example 1: This comparative example does not contain a curing accelerator, but the remaining steps are the same as in Example 1.
[0065] Comparative Example 2: This comparative example uses modified filler instead of reinforced filler, but the other steps are the same as in Example 1.
[0066] Comparative Example 3: This comparative example uses cellulose instead of the modified filler compared to Example 1, but the other steps are the same.
[0067] The colored sand self-leveling floor coatings prepared in Examples 1-3 and Comparative Examples 1-3 were made into test panels according to the standard GB / T22374-2018. After being placed for 7 days, the dry film thickness was 1 mm. The pencil hardness, abrasion resistance and water resistance were tested. The impact resistance was tested using a 1000g steel ball with a height of 100mm. The test results are shown in Table 1 below.
[0068] Table 1
[0069]
[0070] As shown in the table above, this application has excellent wear resistance and water resistance.
[0071] The above description is merely an example and illustration of the concept of the present invention. Those skilled in the art can make various modifications or additions to the specific embodiments described or use similar methods to replace them, as long as they do not deviate from the concept of the invention or exceed the scope defined in the claims, they should all fall within the protection scope of the present invention.
Claims
1. A method for preparing a colored sand self-leveling floor coating, characterized in that: Includes the following steps: Step A1: Cashew phenol, potassium carbonate, allyl chloride and toluene are mixed and reacted to obtain intermediate 1. Intermediate 1, tetramethylcyclotetrasiloxane, chloroplatinic acid and DMF are mixed evenly, and nitrogen gas is introduced for protection to carry out the reaction to obtain intermediate 2. Step A2: Mix intermediate 2, octamethylcyclotetrasiloxane, tetramethylammonium hydroxide, 1,3-bis(3-aminopropyl)-1,1,3,3-tetramethyldisiloxane and dimethyl sulfoxide evenly, purge with nitrogen gas, and react to obtain a curing accelerator. Disperse the modified filler in ethanol, stir, add KH560 and deionized water, and react to obtain a reinforced filler. Step A3: Weigh the following raw materials by weight: 80-90 parts epoxy resin E-51, 10-20 parts reinforcing filler and 10-20 parts 501A epoxy reactive diluent, mix them evenly to obtain component A. Weigh the following raw materials by weight: 15-20 parts curing agent, 5-10 parts curing accelerator, 100-150 parts colored sand, 2-5 parts talc powder, 0.3-1 part dispersant, 0.3-0.5 parts defoamer and 5-10 parts leveling agent, mix them evenly to obtain component B. Mix component A and component B to obtain colored sand self-leveling floor coating. The molar ratio of cashew phenol, potassium carbonate and allyl chloride in step A1 is 1:1.1:1, and the molar ratio of intermediate 1 and tetramethylcyclotetrasiloxane is 1:
4. The molar ratio of intermediate 2, octamethylcyclotetrasiloxane, tetramethylammonium hydroxide and 1,3-bis(3-aminopropyl)-1,1,3,3-tetramethyldisiloxane described in step A2 is 1.2:1.2:3:2; The modified filler is prepared by the following steps: Step B1: Disperse cellulose in N,N-dimethylacetamide, purge with nitrogen, stir and add anhydrous lithium chloride, stir, cool and add triethylamine and p-toluenesulfonyl chloride, react to obtain pretreated cellulose, disperse the pretreated cellulose in N,N-dimethylacetamide, stir and add ammonia water, react to obtain aminated cellulose; Step B2: Aminated cellulose, maleic anhydride, triethylamine and N,N-dimethylformamide are mixed and reacted to obtain modified cellulose. Tetramethyltri-3-trifluoropropylcyclotetrasiloxane, octamethylcyclotetrasiloxane, tetramethylammonium hydroxide, 1,3-bis(3-aminopropyl)-1,1,3,3-tetramethyldisiloxane and dimethyl sulfoxide are mixed evenly, and the mixture is subjected to nitrogen protection to carry out the reaction to obtain the modifier. Step B3: Mix the modifier, allyl glycidyl ether and N,N-dimethylformamide to prepare the modified monomer. Mix the modified monomer, modified cellulose, 1-hexene, azobisisobutyronitrile and N,N-dimethylformamide evenly, and carry out the reaction under nitrogen protection to obtain the modified filler. The mass ratio of cellulose, anhydrous lithium chloride, triethylamine and p-toluenesulfonyl chloride in step B1 is 10mg:1mg:1g:5g, and the volume ratio of pretreated cellulose, N,N-dimethylacetamide and ammonia is 1mL:10mL:20mL. The molar ratio of amino groups, maleic anhydride, and triethylamine on the aminated cellulose described in step B2 is 1:1:1.2, and the molar ratio of tetramethyltri-3-trifluoropropylcyclotetrasiloxane, octamethylcyclotetrasiloxane, tetramethylammonium hydroxide, and 1,3-bis(3-aminopropyl)-1,1,3,3-tetramethyldisiloxane is 1.5:0.9:3:
2. The molar ratio of the modifier and allyl glycidyl ether mentioned in step B3 is 1:4, and the ratio of the amount of the modified monomer, modified cellulose and 1-hexene is 60 mmol: 1 g: 40 mmol.
2. The method for preparing a colored sand self-leveling floor coating according to claim 1, characterized in that: The amount of KH560 used in step A2 is 5% of the mass of the modified filler.
3. A colored sand self-leveling floor coating, characterized in that: Prepared according to any one of the preparation methods described in claims 1-2.
Citation Information
Patent Citations
Epoxy flooring coating containing epoxide group organosilicon hybrid, its preparation method and its application
CN102295875A
Aqueous coating material
JP2019038910A