A one-component waterproof coating based on fluorosilicone polyacrylate emulsion and its preparation method and application

Abstract

The present invention discloses a single-component waterproof coating based on fluorosilicone polyacrylate emulsion, and a preparation method and application thereof, and belongs to the technical field of functional polymer materials. The present invention first prepares a polyacrylate emulsion using an acrylic monomer through an emulsion polymerization process, and then obtains a fluorosilicone polyacrylate emulsion component by grafting a fluorosilicone functional monomer with amino, carboxyl, hydroxyl and other groups in the polyacrylate emulsion structure. At the same time, polytetrafluoroethylene plastic powder is introduced in the preparation process of the single-component waterproof coating, and the two together give the single-component waterproof coating based on fluorosilicone polyacrylate emulsion excellent waterproof and hydrophobic properties. The single-component waterproof coating based on fluorosilicone polyacrylate emulsion involved in the present invention can also meet the waterproof and protection requirements of building materials by optimizing and regulating the ratio and composition of the raw materials, and has broad application prospects.

Description

Technical Field

[0001] The invention belongs to the technical field of functional polymer materials, and specifically relates to a one-component waterproof coating based on fluorosilicone polyacrylate emulsion and a preparation method and application thereof. Background Art

[0002] Due to the influence of aggregate ratio, alkali content, pouring technology, shrinkage and aging of concrete products in the later stage, overload and erosion of other natural factors during the construction process, these adverse effects not only affect the long-term service performance of concrete structures, but also lead to subsequent surface cracking, longitudinal and transverse cracks, and oblique cracks. Therefore, in addition to the necessary firmness, construction projects must also do a good job of surface protection. Among them, the waterproofing and anti-leakage of buildings are one of the important factors to measure whether the quality of construction projects is qualified. In addition, the problem of building leakage is not only a key factor affecting the durability and service life of the construction project structure, but also brings many adverse effects to people, such as personal safety hazards, property losses and inconvenience in life. Finally, compared with demolition and reconstruction, necessary surface protection of buildings can save investment, shorten construction period, and have significant economic and social benefits.

[0003] Although polymer-based building materials waterproof and repair coatings (coatings) have good water resistance, compressive strength, flexibility and adhesion properties, long-term experimental research and waterproof engineering practice have shown that polymer-based building materials waterproof and repair coatings (coatings) have the same waterproof performance as traditional waterproof coatings, and their waterproof durability is poor. Especially in high temperature and high humidity environments, the coatings are prone to absorb water and swell, resulting in the waterproof coating falling off, cracking, and decreased waterproof performance. As the base film-forming resin of waterproof coatings, the performance of polymer emulsions directly determines the waterproof and anti-seepage properties of waterproof coatings. Currently, commercially available polymer emulsions are mainly divided into styrene-acrylic, pure acrylic and acetic acid-acrylic emulsions. Due to the large differences in synthesis process, molecular weight distribution and particle size between different types of emulsions, the performance of polymer waterproof coatings of different emulsion systems is also significantly different. Therefore, the present invention aims at the core problem of high water absorption of waterproof and repair coatings (paints) of polymer-based building materials, and starts with the design and preparation of functional modified polymer emulsions to design and obtain a one-component waterproof coating based on fluorosilicone polyacrylate emulsion and a preparation method thereof. The application mainly involves waterproofing and protection in the field of building materials. Summary of the invention

[0004] The present invention aims at the problems existing in the prior art. The primary purpose of the present invention is to provide a one-component waterproof coating based on fluorosilicone polyacrylate emulsion; secondly, the purpose of the present invention is to provide a one-component waterproof coating based on fluorosilicone polyacrylate emulsion and a preparation method thereof; finally, the purpose of the present invention is to provide an application of the one-component waterproof coating based on fluorosilicone polyacrylate emulsion in the field of waterproofing and protection of building materials.

[0005] In order to achieve the above technical objectives, the technical solution adopted by the present invention is:

[0006] The present invention starts with the design and preparation of polymer emulsion. Firstly, polyacrylate emulsion is prepared by emulsion polymerization process using acrylic acid (ester) monomers. Then, a fluorosilicone polyacrylate emulsion component is obtained by grafting fluorosilicone functional monomers with amino, carboxyl and hydroxyl groups in the polyacrylate emulsion structure. Then, inorganic components and auxiliary components (dispersant, defoamer, bactericidal and mildewproof agent, thickener and dye paste) are added to prepare a single-component waterproof coating based on fluorosilicone polyacrylate emulsion.

[0007] A one-component waterproof coating based on fluorosilicone polyacrylate emulsion is prepared by including the following raw materials in parts by weight: 15-50 parts of fluorosilicone polyacrylate emulsion component, 20-50 parts of filler component, 0.5-1 part of dispersant, 1-1.5 parts of defoamer, 0.5-1 part of bactericide and mildewproof agent, 0.5-1 part of thickener, 1-3 parts of dye paste and 20-40 parts of deionized water.

[0008] A one-component waterproof coating based on fluorosilicone polyacrylate emulsion is prepared by including the following raw materials in parts by weight: 35-40 parts of fluorosilicone polyacrylate emulsion component, 45-48 parts of filler component, 0.5-1 part of dispersant, 1-1.5 parts of defoamer, 0.5-1 part of bactericide and mildewproof agent, 0.5-1 part of thickener, 1-3 parts of dye paste and 20-30 parts of deionized water.

[0009] Furthermore, the fluorosilicone polyacrylate emulsion component is prepared by including the following raw materials in parts by weight: 98-100 parts of acrylic monomer, 1-10 parts of fluorosilicone functional monomer, 1-4 parts of emulsifier, 0.5-1.5 parts of initiator, and 120-130 parts of deionized water.

[0010] Furthermore, the fluorosilicone polyacrylate emulsion component is prepared by including the following raw materials in parts by weight: 98-100 parts of acrylic monomer, 1-5 parts of fluorine-silicone functional monomer, 1-3 parts of emulsifier, 0.5-1 part of initiator, and 120-130 parts of deionized water.

[0011] Furthermore, the acrylic monomer is a combination of acrylic acid, methacrylic acid, methyl methacrylate, ethyl acrylate, butyl acrylate, methacryloxypropyltrimethoxysilane, glycidyl methacrylate, hydroxyethyl acrylate, hydroxypropyl acrylate, and hydroxybutyl acrylate.

[0012] Furthermore, the acrylic monomer is one or more of acrylic acid, methyl methacrylate, butyl acrylate, hydroxybutyl acrylate, hydroxyethyl acrylate, and glycidyl methacrylate.

[0013] Furthermore, the fluorosilicone functional monomer is one or more of trifluoroacetic acid, octafluoropentanoic acid, tetrafluoropropionic acid, perfluorooctanoic acid, γ-aminopropyltriethoxysilane KH-550, γ-glycidyloxypropyltrimethoxysilane KH-560, and 3-isocyanate ester propyltriethoxysilane.

[0014] Furthermore, the fluorine-containing functional monomer is one or more of octafluoropentanoic acid, perfluorooctanoic acid, γ-aminopropyltriethoxysilane KH-550, γ-glycidyloxypropyltrimethoxysilane KH-560, and 3-isocyanate ester propyltriethoxysilane.

[0015] Furthermore, the emulsifier is one or more of nonylphenol polyoxyethylene ether ammonium sulfate, alkyl alcohol alkoxylated sulfate sodium salt, nonylphenol ethoxylated sulfate ammonium salt, alkyl alcohol ethoxylated sulfate sodium salt, sodium dodecyl sulfate, sodium dodecylbenzene sulfonate, allyloxy nonylphenol polyoxyethylene ether ammonium sulfate, and sodium vinyl sulfonate.

[0016] Furthermore, the emulsifier is alkyl alcohol alkoxylated sodium sulfate AS801 and / or sodium vinyl sulfonate.

[0017] Furthermore, the initiator is one of ammonium persulfate, potassium persulfate and sodium persulfate.

[0018] Furthermore, the initiator is one of ammonium persulfate and potassium persulfate.

[0019] Furthermore, the preparation method of the fluorosilicone polyacrylate emulsion component of the present invention is a pre-emulsification polymerization process, comprising the following steps:

[0020] (1) preparing various raw materials by weight, then adding an emulsifier and 40% deionized water into a pre-emulsification kettle, and then adding an initiator, stirring and mixing evenly, adding an acrylic monomer into the pre-emulsification kettle, and emulsifying for 0.5-1h to obtain a pre-emulsified liquid;

[0021] (2) Then, the remaining 60% of deionized water was added to the polymerization reactor, and the temperature was raised to 80° C. with stirring, and the pre-emulsion was added dropwise, and the dropping time was controlled to be 3.5-4 h. After the dropping was completed, the temperature was raised to 90° C., and the temperature was kept for reaction for 1 h, and then the temperature was lowered to 70° C., and the fluorine-containing silicon functional monomer was added, and the reaction was continued for 0.5-1.0 h, and then the reaction was terminated. After the temperature was lowered to 30-40° C., the pH value was adjusted to 7-8 with ammonia water, and then 0.25 parts by weight of tert-butyl hydroperoxide and 0.25 parts by weight of Rongalite were added in sequence to remove the residual acrylic acid monomer in the system, and finally 0.5 parts by weight of a wetting agent and 0.3 parts by weight of a defoaming agent were added, and the mixture was filtered through a 120-mesh filter to remove impurities, and the mixture was obtained.

[0022] The filler component is a combination of 400 mesh heavy calcium, 400 mesh quartz sand, and 400 mesh polytetrafluoroethylene plastic powder; the dispersant is a polycarboxylate dispersing water-reducing agent 5040; the defoamer is a mineral oil defoamer (NXZ (Nopco)) and / or a silicone defoamer (BYK-028 (BYK)); the thickener is one of thickeners ASE60 (Dow) or L344 (Aksu); the dye paste is one of phthalocyanine blue, iron red, chrome yellow, and carbon black paste.

[0023] A preparation method of a one-component waterproof coating based on fluorosilicone polyacrylate emulsion comprises the following preparation steps: firstly, a filler component is mixed with deionized water, a dispersant and a defoamer are added in sequence during the stirring process, and after the stirring is uniform, a fluorosilicone polyacrylate emulsion component is added, stirring is carried out for 10 minutes, a bactericide and mildew preventer are added, and then a thickener is added to adjust the viscosity of the system, and finally a dye paste is added, and stirring is continued for 20 minutes to obtain the one-component waterproof coating.

[0024] An application of a one-component waterproof coating based on fluorosilicone polyacrylate emulsion, which is applied in the field of waterproofing and protection of building materials.

[0025] Beneficial Effects

[0026] (1) The present invention first prepares a polyacrylate emulsion using an acrylic monomer through an emulsion polymerization process, and then obtains a fluorosilicone polyacrylate emulsion component by grafting fluorosilicone functional monomers with amino, carboxyl and hydroxyl groups in the polyacrylate emulsion structure. At the same time, polytetrafluoroethylene plastic powder is introduced into the preparation process of the single-component waterproof coating. The two together give the single-component waterproof coating based on the fluorosilicone polyacrylate emulsion excellent waterproof and hydrophobic properties;

[0027] (2) The one-component waterproof coating based on fluorosilicone polyacrylate emulsion of the present invention can also meet the waterproof and protection requirements of building materials by optimizing and regulating the ratio and composition of the raw materials, and has broad application prospects. DETAILED DESCRIPTION

[0028] The technical solution of the present invention is further described below in conjunction with specific examples, but is not limited thereto. Examples 1-8 are the preparation of fluorosilicone polyacrylate emulsions, and Examples 9-18 are the preparation of single-component waterproof coatings based on fluorosilicone polyacrylate emulsions, but the embodiments of the present invention are not limited thereto.

[0029] Example 1

[0030] The preparation method of the fluorosilicone polyacrylate emulsion component is:

[0031] 1 kg of alkyl alcohol alkoxylated sodium sulfate (AS801), 1.5 kg of sodium vinyl sulfonate, 50 kg of deionized water and 0.5 kg of potassium persulfate initiator were stirred and mixed, and then 4 kg of acrylic acid, 16 kg of methyl methacrylate, 70 kg of butyl acrylate, 5 kg of hydroxyethyl acrylate and 3 kg of glycidyl methacrylate were added in sequence, and emulsified for 0.5-1 hour to obtain a pre-emulsion. Then, 75 kg of deionized water was added to the polymerization kettle, and the mixture was stirred and heated to 80° C., and then the pre-emulsion was added dropwise, and the dropping time was controlled to be 3.5-4 h. After the dropping was completed, the mixture was heated to 90° C. and kept warm for reaction for 1 h. Then the mixture was cooled to 70° C., and then 2 kg of octafluoropentanoic acid was added. The reaction was continued for 0.5-1.0 h, and then the reaction was terminated and the temperature was cooled to 30-40° C. The pH value was adjusted to 7-8 with 3 kg of ammonia water, and then 0.25 kg of tert-butyl hydroperoxide and 0.25 kg of Rongalite were added in sequence to remove residual acrylic monomers. Finally, 0.5 kg of wetting agent (OT-75) and 0.3 kg of defoaming agent (691) were added, and the mixture was filtered through a 120-mesh filter to remove impurities, thereby obtaining a fluorosilicone polyacrylate emulsion.

[0032] Example 2

[0033] The preparation method of the fluorosilicone polyacrylate emulsion component is as follows: 1 kg of alkyl alcohol alkoxylated sodium sulfate (AS801), 1.5 kg of sodium vinyl sulfonate, 50 kg of deionized water and 0.5 kg of potassium persulfate initiator are stirred and mixed, and then 4 kg of acrylic acid, 16 kg of methyl methacrylate, 70 kg of butyl acrylate, 5 kg of hydroxyethyl acrylate and 3 kg of glycidyl methacrylate are added in sequence, and emulsified for 0.5-1 hour to obtain a pre-emulsion. Then, 75 kg of deionized water was added to the polymerization kettle, and the mixture was stirred and heated to 80° C., and then the pre-emulsion was added dropwise, and the dropping time was controlled to be 3.5-4 h. After the dropping was completed, the mixture was heated to 90° C. and kept warm for reaction for 1 h. Then the mixture was cooled to 70° C., and then 2 kg of perfluorooctanoic acid was added. The reaction was continued for 0.5-1.0 h, and then the reaction was terminated and the temperature was cooled to 30-40° C. The pH value was adjusted to 7-8 with 3 kg of ammonia water, and then 0.25 kg of tert-butyl hydroperoxide and 0.25 kg of Rongalite were added in sequence to remove residual acrylic monomers. Finally, 0.5 kg of wetting agent (OT-75) and 0.3 kg of defoaming agent (691) were added, and the mixture was filtered through a 120-mesh filter to remove impurities, thereby obtaining a fluorosilicone polyacrylate emulsion.

[0034] Example 3

[0035] The preparation method of the fluorosilicone polyacrylate emulsion component is:

[0036] A preparation method of a fluorosilicone polyacrylate emulsion is as follows: 1 kg of alkyl alcohol alkoxylated sodium sulfate (AS801), 1.5 kg of sodium vinyl sulfonate, 50 kg of deionized water and 0.5 kg of potassium persulfate initiator are stirred and mixed, and then 4 kg of acrylic acid, 16 kg of methyl methacrylate, 70 kg of butyl acrylate, 5 kg of hydroxyethyl acrylate and 3 kg of glycidyl methacrylate are added in sequence, and emulsified for 0.5-1 hour to obtain a pre-emulsion. Then, 75 kg of deionized water was added to the polymerization kettle, and the mixture was stirred and heated to 80°C, and then the pre-emulsion was added dropwise, and the dropping time was controlled to be 3.5-4 h. After the dropping was completed, the mixture was heated to 90°C and kept for reaction for 1 h, and then cooled to 70°C, and then 3 kg of γ-aminopropyltriethoxysilane (KH-550) was added, and the reaction was continued for 0.5-1.0 h, and then the reaction was terminated and the temperature was cooled to 30-40°C. The pH value was adjusted to 7-8 with 3 kg of ammonia water, and then 0.25 kg of tert-butyl hydroperoxide and 0.25 kg of Rongalite were added in sequence to remove residual acrylic monomers, and finally 0.5 kg of wetting agent (OT-75) and 0.3 kg of defoaming agent (691) were added, and the mixture was filtered through a 120-mesh filter to remove impurities, thereby obtaining a fluorosilicone polyacrylate emulsion.

[0037] Example 4

[0038] The preparation method of the fluorosilicone polyacrylate emulsion component is:

[0039] 1 kg of alkyl alcohol alkoxylated sodium sulfate (AS801), 1.5 kg of sodium vinyl sulfonate, 50 kg of deionized water and 0.5 kg of potassium persulfate initiator were stirred and mixed, and then 4 kg of acrylic acid, 16 kg of methyl methacrylate, 70 kg of butyl acrylate, 5 kg of hydroxyethyl acrylate and 3 kg of glycidyl methacrylate were added in sequence, and emulsified for 0.5-1 hour to obtain a pre-emulsion. Then, 75 kg of deionized water was added to the polymerization kettle, and the mixture was stirred and heated to 80°C, and then the pre-emulsion was added dropwise, and the dropping time was controlled to be 3.5-4 h. After the dropping was completed, the mixture was heated to 90°C and kept for reaction for 1 h, and then cooled to 70°C, and then 3 kg of γ-glycidyloxypropyltrimethoxysilane (KH-560) was added, and the reaction was continued for 0.5-1.0 h, and then the reaction was terminated and the temperature was cooled to 30-40°C. The pH value was adjusted to 7-8 with 3 kg of ammonia water, and then 0.25 kg of tert-butyl hydroperoxide and 0.25 kg of Rongalite were added in sequence to remove residual acrylic monomers, and finally 0.5 kg of wetting agent (OT-75) and 0.3 kg of defoaming agent (691) were added, and the mixture was filtered through a 120-mesh filter to remove impurities, thereby obtaining a fluorosilicone polyacrylate emulsion.

[0040] Example 5

[0041] The preparation method of the fluorosilicone polyacrylate emulsion component is:

[0042] A preparation method of a fluorosilicone polyacrylate emulsion is as follows: 1 kg of alkyl alcohol alkoxylated sodium sulfate (AS801), 1.5 kg of sodium vinyl sulfonate, 50 kg of deionized water and 0.5 kg of potassium persulfate initiator are stirred and mixed, and then 4 kg of acrylic acid, 16 kg of methyl methacrylate, 70 kg of butyl acrylate, 5 kg of hydroxyethyl acrylate and 3 kg of glycidyl methacrylate are added in sequence, and emulsified for 0.5-1 hour to obtain a pre-emulsion. Then, 75 kg of deionized water was added to the polymerization kettle, and the mixture was stirred and heated to 80° C., and then the pre-emulsion was added dropwise, and the dropping time was controlled to be 3.5-4 h. After the dropping was completed, the mixture was heated to 90° C. and kept warm for reaction for 1 h. Then, the mixture was cooled to 70° C., and then 1 kg of perfluorooctanoic acid and 2 kg of γ-glycidyloxypropyltrimethoxysilane (KH-560) were added. The reaction was continued for 0.5-1.0 h, and then the reaction was terminated and the temperature was cooled to 30-40° C. The pH value was adjusted to 7-8 with 3 kg of ammonia water, and then 0.25 kg of tert-butyl hydroperoxide and 0.25 kg of Rongalite were added in sequence to remove residual acrylic monomers. Finally, 0.5 kg of wetting agent (OT-75) and 0.3 kg of defoaming agent (691) were added, and the mixture was filtered through a 120-mesh filter to remove impurities, thereby obtaining a fluorosilicone polyacrylate emulsion.

[0043] Example 6

[0044] The preparation method of the fluorosilicone polyacrylate emulsion component is:

[0045] A preparation method of a fluorosilicone polyacrylate emulsion is as follows: 1 kg of alkyl alcohol alkoxylated sodium sulfate (AS801), 1.5 kg of sodium vinyl sulfonate, 50 kg of deionized water and 0.5 kg of potassium persulfate initiator are stirred and mixed, and then 4 kg of acrylic acid, 16 kg of methyl methacrylate, 70 kg of butyl acrylate, 5 kg of hydroxyethyl acrylate and 3 kg of glycidyl methacrylate are added in sequence, and emulsified for 0.5-1 hour to obtain a pre-emulsion. Then, 75 kg of deionized water was added to the polymerization kettle, and the mixture was stirred and heated to 80° C., and then the pre-emulsion was added dropwise, and the dropping time was controlled to be 3.5-4 h. After the dropping was completed, the mixture was heated to 90° C. and kept warm for reaction for 1 h. Then, the mixture was cooled to 70° C., and then 1 kg of perfluorooctanoic acid and 1 kg of 3-isocyanate propyltriethoxysilane were added. The reaction was continued for 0.5-1.0 h, and then the reaction was terminated and the temperature was cooled to 30-40° C. The pH value was adjusted to 7-8 with 3 kg of ammonia water, and then 0.25 kg of tert-butyl hydroperoxide and 0.25 kg of Rongalite were added in sequence to remove residual acrylic monomers. Finally, 0.5 kg of wetting agent (OT-75) and 0.3 kg of defoaming agent (691) were added, and the mixture was filtered through a 120-mesh filter to remove impurities, thereby obtaining a fluorosilicone polyacrylate emulsion.

[0046] Example 7

[0047] The preparation method of the fluorosilicone polyacrylate emulsion component is:

[0048] A preparation method of a fluorosilicone polyacrylate emulsion is as follows: 1 kg of alkyl alcohol alkoxylated sodium sulfate (AS801), 2 kg of sodium vinyl sulfonate, 52 kg of deionized water and 1.5 kg of potassium persulfate initiator are stirred and mixed, and then 4 kg of acrylic acid, 16 kg of methyl methacrylate, 70 kg of butyl acrylate, 5 kg of hydroxyethyl acrylate and 4 kg of glycidyl methacrylate are added in sequence, and emulsified for 0.5-1 hour to obtain a pre-emulsion. Then, 78 kg of deionized water was added to the polymerization kettle, and the mixture was stirred and heated to 80° C., and then the pre-emulsion was added dropwise, and the dropping time was controlled to be 3.5-4 h. After the dropping was completed, the mixture was heated to 90° C. and kept warm for reaction for 1 h. Then, the mixture was cooled to 70° C., and then 2.5 kg of perfluorooctanoic acid and 2.5 kg of 3-isocyanate propyltriethoxysilane were added. The reaction was continued for 0.5-1.0 h, and then the reaction was terminated and the temperature was cooled to 30-40° C. The pH value was adjusted to 7-8 with 3 kg of ammonia water, and then 0.25 kg of tert-butyl hydroperoxide and 0.25 kg of Rongalite were added in sequence to remove residual acrylic monomers. Finally, 0.5 kg of wetting agent (OT-75) and 0.3 kg of defoaming agent (691) were added, and the mixture was filtered through a 120-mesh filter to remove impurities, thereby obtaining a fluorosilicone polyacrylate emulsion.

[0049] Example 8

[0050] The preparation method of the fluorosilicone polyacrylate emulsion component is:

[0051] A preparation method of a fluorosilicone polyacrylate emulsion is as follows: 1 kg of alkyl alcohol alkoxylated sodium sulfate (AS801), 48 kg of deionized water and 0.5 kg of potassium persulfate initiator are stirred and mixed, and then 4 kg of acrylic acid, 16 kg of methyl methacrylate, 70 kg of butyl acrylate and 4 kg of hydroxyethyl acrylate, 4 kg of glycidyl methacrylate are added in sequence, and emulsified for 0.5-1 hour to obtain a pre-emulsion. Then, 72 kg of deionized water was added to the polymerization kettle, and the mixture was stirred and heated to 80° C., and then the pre-emulsion was added dropwise, and the dropping time was controlled to be 3.5-4 h. After the dropping was completed, the mixture was heated to 90° C. and kept warm for reaction for 1 h. Then the mixture was cooled to 70° C., and then 1 kg of perfluorooctanoic acid was added. The reaction was continued for 0.5-1.0 h, and then the reaction was terminated and the temperature was cooled to 30-40° C. The pH value was adjusted to 7-8 with 3 kg of ammonia water, and then 0.25 kg of tert-butyl hydroperoxide and 0.25 kg of Rongalite were added in sequence to remove residual acrylic monomers. Finally, 0.5 kg of wetting agent (OT-75) and 0.3 kg of defoaming agent (691) were added, and the mixture was filtered through a 120-mesh filter to remove impurities, thereby obtaining a fluorosilicone polyacrylate emulsion.

[0052] Example 9

[0053] A preparation method of a one-component waterproof coating based on a fluorosilicone polyacrylate emulsion comprises the following steps: firstly, 30kg of heavy calcium (400 mesh), 10kg of quartz sand (400 mesh), 5kg of polytetrafluoroethylene plastic powder (400 mesh) and 25kg of deionized water are mixed, 0.8kg of a dispersant (5040) and 1kg of a defoamer (BYK-028) are added in sequence during the stirring process, 35kg of a fluorosilicone polyacrylate emulsion (Example 1) is added after being stirred evenly, the mixture is stirred for 10 minutes, 0.5kg of a Kathon bactericidal and mildewproof agent is added, 0.8kg of an ASE60 thickener is then added to adjust the viscosity of the system, and finally 0.4kg of a phthalocyanine blue slurry is added, and the stirring is continued for 20 minutes to obtain the one-component waterproof coating of the fluorosilicone polyacrylate emulsion.

[0054] Example 10

[0055] A preparation method of a one-component waterproof coating based on a fluorosilicone polyacrylate emulsion comprises the following steps: firstly, 30kg of heavy calcium (400 mesh), 10kg of quartz sand (400 mesh), 5kg of polytetrafluoroethylene plastic powder (400 mesh) and 25kg of deionized water are mixed, 0.8kg of a dispersant (5040) and 1kg of a defoamer (BYK-028) are added in sequence during the stirring process, 35kg of a fluorosilicone polyacrylate emulsion (Example 2) is added after being stirred evenly, stirring for 10 minutes, 0.5kg of a Kathon bactericidal and mildewproof agent is added, then 0.8kg of an ASE60 thickener is added to adjust the viscosity of the system, and finally 0.4kg of a phthalocyanine blue slurry is added, and stirring is continued for 20 minutes to obtain the one-component waterproof coating of the fluorosilicone polyacrylate emulsion.

[0056] Embodiment 11

[0057] A preparation method of a one-component waterproof coating based on a fluorosilicone polyacrylate emulsion comprises the following steps: firstly, 30kg of heavy calcium (400 mesh), 10kg of quartz sand (400 mesh), 5kg of polytetrafluoroethylene plastic powder (400 mesh) and 25kg of deionized water are mixed, 0.8kg of a dispersant (5040) and 1kg of a defoamer (BYK-028) are added in sequence during the stirring process, 35kg of a fluorosilicone polyacrylate emulsion (Example 3) is added after being stirred evenly, stirring for 10 minutes, 0.5kg of a Kathon bactericidal and mildewproof agent is added, then 0.8kg of an ASE60 thickener is added to adjust the viscosity of the system, and finally 0.4kg of a phthalocyanine blue slurry is added, and stirring is continued for 20 minutes to obtain the one-component waterproof coating of the fluorosilicone polyacrylate emulsion.

[0058] Example 12

[0059] A preparation method of a one-component waterproof coating based on a fluorosilicone polyacrylate emulsion comprises the following steps: firstly, 30kg of heavy calcium (400 mesh), 10kg of quartz sand (400 mesh), 5kg of polytetrafluoroethylene plastic powder (400 mesh) and 25kg of deionized water are mixed, 0.8kg of a dispersant (5040) and 1kg of a defoamer (BYK-028) are added in sequence during the stirring process, 35kg of a fluorosilicone polyacrylate emulsion (Example 4) is added after being stirred evenly, the mixture is stirred for 10 minutes, 0.5kg of a Kathon bactericidal and mildewproof agent is added, 0.8kg of an ASE60 thickener is then added to adjust the viscosity of the system, and finally 0.4kg of a phthalocyanine blue slurry is added, and stirring is continued for 20 minutes to obtain the one-component waterproof coating of the fluorosilicone polyacrylate emulsion.

[0060] Example 13

[0061] A preparation method of a one-component waterproof coating based on a fluorosilicone polyacrylate emulsion comprises the following steps: firstly, 30kg of heavy calcium (400 mesh), 10kg of quartz sand (400 mesh), 5kg of polytetrafluoroethylene plastic powder (400 mesh) and 25kg of deionized water are mixed, 0.8kg of a dispersant (5040) and 1kg of a defoamer (BYK-028) are added in sequence during the stirring process, 35kg of a fluorosilicone polyacrylate emulsion (Example 5) is added after being stirred evenly, the mixture is stirred for 10 minutes, 0.5kg of a Kathon bactericidal and mildewproof agent is added, 0.8kg of an ASE60 thickener is then added to adjust the viscosity of the system, and finally 0.4kg of a phthalocyanine blue slurry is added, and stirring is continued for 20 minutes to obtain the one-component waterproof coating of the fluorosilicone polyacrylate emulsion.

[0062] Embodiment 14

[0063] A preparation method of a one-component waterproof coating based on a fluorosilicone polyacrylate emulsion comprises the following steps: firstly, 30kg of heavy calcium (400 mesh), 10kg of quartz sand (400 mesh), 5kg of polytetrafluoroethylene plastic powder (400 mesh) and 25kg of deionized water are mixed, 0.8kg of a dispersant (5040) and 1kg of a defoamer (BYK-028) are added in sequence during the stirring process, 35kg of a fluorosilicone polyacrylate emulsion (Example 6) is added after being stirred evenly, the mixture is stirred for 10 minutes, 0.5kg of a Kathon bactericidal and mildewproof agent is added, 0.8kg of an ASE60 thickener is then added to adjust the viscosity of the system, and finally 0.4kg of a phthalocyanine blue slurry is added, and stirring is continued for 20 minutes to obtain the one-component waterproof coating of the fluorosilicone polyacrylate emulsion.

[0064] Embodiment 15

[0065] A preparation method of a one-component waterproof coating based on a fluorosilicone polyacrylate emulsion comprises the following steps: firstly, 30kg of heavy calcium (400 mesh), 10kg of quartz sand (400 mesh), 5kg of polytetrafluoroethylene plastic powder (400 mesh) and 25kg of deionized water are mixed, 0.8kg of a dispersant (5040) and 1kg of a defoamer (BYK-028) are added in sequence during the stirring process, 40kg of a fluorosilicone polyacrylate emulsion (Example 5) is added after being stirred evenly, stirring for 10 minutes, 0.5kg of a Kathon bactericidal and mildewproof agent is added, then 0.8kg of an ASE60 thickener is added to adjust the viscosity of the system, and finally 0.4kg of a phthalocyanine blue slurry is added, and stirring is continued for 20 minutes to obtain the one-component waterproof coating of the fluorosilicone polyacrylate emulsion.

[0066] Example 16

[0067] A preparation method of a one-component waterproof coating based on a fluorosilicone polyacrylate emulsion comprises the following steps: firstly, 30kg of heavy calcium (400 mesh), 10kg of quartz sand (400 mesh), 8kg of polytetrafluoroethylene plastic powder (400 mesh) and 25kg of deionized water are mixed, 0.8kg of a dispersant (5040) and 1kg of a defoamer (BYK-028) are added in sequence during the stirring process, 35kg of a fluorosilicone polyacrylate emulsion (Example 5) is added after being stirred evenly, the mixture is stirred for 10 minutes, 0.5kg of a Kathon bactericidal and mildewproof agent is added, 0.8kg of an ASE60 thickener is then added to adjust the viscosity of the system, and finally 0.4kg of a phthalocyanine blue slurry is added, and stirring is continued for 20 minutes to obtain the one-component waterproof coating of the fluorosilicone polyacrylate emulsion.

[0068] Embodiment 17

[0069] A preparation method of a one-component waterproof coating based on a fluorosilicone polyacrylate emulsion comprises the following steps: firstly, 30kg of heavy calcium (400 mesh), 10kg of quartz sand (400 mesh), 5kg of polytetrafluoroethylene plastic powder (400 mesh) and 25kg of deionized water are mixed, 0.8kg of a dispersant (5040) and 1kg of a defoamer (BYK-028) are added in sequence during the stirring process, 35kg of a fluorosilicone polyacrylate emulsion (Example 7) is added after being stirred evenly, the mixture is stirred for 10 minutes, 0.5kg of a Kathon bactericidal and mildewproof agent is added, 0.8kg of an ASE60 thickener is then added to adjust the viscosity of the system, and finally 0.4kg of iron red slurry is added, and stirring is continued for 20 minutes to obtain the one-component waterproof coating of the fluorosilicone polyacrylate emulsion.

[0070] Embodiment 18

[0071] A preparation method of a one-component waterproof coating based on a fluorosilicone polyacrylate emulsion comprises the following steps: firstly, 30kg of heavy calcium (400 mesh), 10kg of quartz sand (400 mesh), 5kg of polytetrafluoroethylene plastic powder (400 mesh) and 25kg of deionized water are mixed, 0.8kg of a dispersant (5040) and 1kg of a defoamer (BYK-028) are added in sequence during the stirring process, 35kg of a fluorosilicone polyacrylate emulsion (Example 8) is added after being stirred evenly, the mixture is stirred for 10 minutes, 0.5kg of a Kathon bactericidal and mildewproof agent is added, 0.8kg of an ASE60 thickener is then added to adjust the viscosity of the system, and finally 0.4kg of a chrome yellow slurry is added, and the stirring is continued for 20 minutes to obtain the one-component waterproof coating of the fluorosilicone polyacrylate emulsion.

[0072] Comparative Example 1

[0073] A preparation method of a fluorosilicone polyacrylate emulsion is as follows: 1 kg of alkyl alcohol alkoxylated sodium sulfate (AS801), 2 kg of sodium vinyl sulfonate, 52 kg of deionized water and 1.5 kg of potassium persulfate initiator are stirred and mixed, and then 4 kg of acrylic acid, 16 kg of methyl methacrylate, 70 kg of butyl acrylate, 5 kg of hydroxyethyl acrylate and 4 kg of glycidyl methacrylate are added in sequence, and emulsified for 0.5-1 hour to obtain a pre-emulsion. Then, 78 kg of deionized water was added to the polymerization kettle, and the mixture was stirred and heated to 80° C., and then the pre-emulsion was added dropwise, and the dropping time was controlled to be 3.5-4 h. After the dropping was completed, the mixture was heated to 90° C. and kept warm for 2 h to terminate the reaction. The mixture was cooled to 30-40° C., and the pH value was adjusted to 7-8 with 3 kg of ammonia water. Then, 0.25 kg of tert-butyl hydroperoxide and 0.25 kg of Rongalite were added in sequence to remove residual acrylic monomers. Finally, 0.5 kg of wetting agent (OT-75) and 0.3 kg of defoaming agent (691) were added, and the mixture was filtered through a 120-mesh filter to remove impurities, thereby obtaining a fluorosilicone polyacrylate emulsion.

[0074] Comparative Example 2

[0075] A method for preparing a polyacrylate emulsion one-component waterproof coating comprises the following steps: firstly, 30kg of heavy calcium (400 mesh), 10kg of quartz sand (400 mesh) and 25kg of deionized water are mixed, 0.8kg of a dispersant (5040) and 1kg of a defoamer (BYK-028) are added in sequence during the stirring process, 35kg of a polyacrylate emulsion (Comparative Example 1) is added after being stirred evenly, stirring for 10 minutes, 0.5kg of a Kathon bactericidal and mildewproof agent is added, then 0.8kg of an ASE60 thickener is added to adjust the viscosity of the system, and finally 0.4kg of a phthalocyanine blue slurry is added, and stirring is continued for 20 minutes to obtain a fluorosilicone polyacrylate emulsion one-component waterproof coating.

[0076] Comparative Example 3

[0077] A method for preparing a polyacrylate emulsion one-component waterproof coating comprises the following steps: firstly, 30kg of heavy calcium (400 mesh), 10kg of quartz sand (400 mesh), 5kg of polytetrafluoroethylene plastic powder (400 mesh) and 25kg of deionized water are mixed, 0.8kg of a dispersant (5040) and 1kg of a defoamer (BYK-028) are added in sequence during the stirring process, 35kg of polyacrylate emulsion (Comparative Example 1) is added after being stirred evenly, stirring for 10 minutes, 0.5kg of a Kathon bactericidal and mildewproof agent is added, then 0.8kg of an ASE60 thickener is added to adjust the viscosity of the system, and finally 0.4kg of a phthalocyanine blue slurry is added, and stirring is continued for 20 minutes to obtain a fluorosilicone polyacrylate emulsion one-component waterproof coating.

[0078] Comparative Example 4

[0079] A preparation method of a one-component waterproof coating based on a fluorosilicone polyacrylate emulsion comprises the following steps: firstly, 30kg of heavy calcium (400 mesh), 10kg of quartz sand (400 mesh) and 25kg of deionized water are mixed, 0.8kg of a dispersant (5040) and 1kg of a defoamer (BYK-028) are added in sequence during the stirring process, 35kg of a fluorosilicone polyacrylate emulsion (Example 7) is added after being stirred evenly, stirring for 10 minutes, 0.5kg of a Kathon bactericidal and mildewproof agent is added, then 0.8kg of an ASE60 thickener is added to adjust the viscosity of the system, and finally 0.4kg of iron red slurry is added, and stirring is continued for 20 minutes to obtain the one-component waterproof coating of the fluorosilicone polyacrylate emulsion.

[0080] Performance Testing

[0081] The particle size and distribution of the fluorosilicone polyacrylate emulsion prepared by the present invention were tested by dynamic light scattering (DLS) measurement (Brookhaven ZetaPlus). Table 1 Intensity particle size and distribution results of the fluorosilicone polyacrylate emulsion prepared by Examples (1-8) of the present invention at a dilution of 1000 times. The results show that the fluorosilicone polyacrylate emulsion prepared by the present invention meets the basic requirements of building waterproof emulsion in terms of appearance, stability and emulsion particle size.

[0082] Table 1 Appearance, stability, particle size and distribution of fluorosilicone polyacrylate emulsion prepared in the embodiment of the present invention

[0083] sample Appearance Particle size (d.nm) and distribution (PDI) Example 1 Milky white, no stratification for six months 188，1.14 Example 2 Milky white, no stratification for six months 175，1.19 Example 3 Milky white, no stratification for six months 180，107 Example 4 Milky white, no stratification for six months 202，1.11 Example 5 Milky white, no stratification for six months 216，1.24 Example 6 Milky white, no stratification for six months 197，1.21 Example 7 Milky white, no stratification for six months 199，1.19 Example 8 Milky white, no stratification for six months 198，1.21 Comparative Example 1 Milky white, no stratification for six months 190，1.11

[0084] In order to evaluate the hydrophobicity and water resistance of the fluorosilicone polyacrylate emulsion, the present invention measured the contact angle of the emulsion coating, and then measured the water absorption rate of the emulsion coating with reference to the industry standard JC / T 1017-2006 "Polymer Emulsion for Building Waterproof Coating". The results show that the fluorosilicone polyacrylate emulsion coating prepared by the present invention has excellent hydrophobicity, and the contact angle of the coating will further improve with the increase of fluorosilicone content; at the same time, the water absorption rate of the coating is also very low, and the water absorption rate of the coating for 72 hours is less than 15%. Studies have shown that the emulsion component is the key component that determines the hydrophobicity and waterproofness of the waterproof coating, and the fluorosilicone polyacrylate emulsion coating prepared by the present invention not only has excellent hydrophobicity, but also has very low water absorption rate, which provides a solid foundation for the excellent hydrophobicity and waterproofness of the subsequent single-component waterproof coating based on the fluorosilicone polyacrylate emulsion.

[0085] Table 2 Contact angle and water absorption of fluorosilicone polyacrylate emulsion coating prepared in the embodiment of the present invention

[0086]

[0087]

[0088] Table 3 Contact angle and water absorption of the one-component waterproof coating film based on fluorosilicone polyacrylate emulsion prepared in the embodiment of the present invention

[0089]

[0090] The performance test of the one-component waterproof coating based on fluorosilicone polyacrylate emulsion prepared by the present invention refers to the standards JC / T2090-2011 "Polymer Cement Waterproof Slurry" and GB / T 23445-2009 "Polymer Cement Waterproof Coating". Table 3 Contact angle and water absorption rate of the one-component waterproof coating film (5 cm (diameter) * 1.5 cm (thickness)) based on fluorosilicone polyacrylate emulsion prepared in the embodiment of the present invention. The results show that the waterproof coating also has low water absorption and excellent hydrophobic properties.

[0091] Table 4 shows the performance of the one-component waterproof coating based on fluorosilicone polyacrylate emulsion prepared in the embodiment of the present invention. The results show that the one-component waterproof coating based on fluorosilicone polyacrylate emulsion has excellent waterproof, anti-seepage, strong adhesion and mechanical properties, and thus has broad application prospects.

[0092] Table 4 Performance of one-component waterproof coating based on fluorosilicone polyacrylate emulsion in the embodiment of the present invention

[0093]

[0094] It should be noted that the above embodiments are only partial embodiments of the preferred methods of implementing the present invention, rather than all embodiments. Obviously, based on the above embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work should fall within the scope of protection of the present invention.

Claims

1. A one-component waterproof coating based on fluorosilicone polyacrylate emulsion, characterized in that: The invention is prepared by the following raw materials in parts by weight: 35-40 parts of fluorosilicone polyacrylate emulsion component, 45-48 parts of filler component, 0.5-1 part of dispersant, 1-1.5 parts of defoamer, 0.5-1 part of bactericide and mildewproof agent, 0.5-1 part of thickener, 1-3 parts of dye paste and 20-30 parts of deionized water; the fluorosilicone polyacrylate emulsion component is prepared by first preparing polyacrylate emulsion by emulsion polymerization of acrylic monomer, and then preparing the polyacrylate emulsion by grafting reaction of fluorosilicone functional monomer and polyacrylate emulsion; the fluorosilicone polyacrylate emulsion component is prepared by the following raw materials in parts by weight: 98-100 parts of acrylic monomer, 1-5 parts of fluorosilicone functional monomer, 1-3 parts of emulsifier, 0.5-1 part of initiator and 120-130 parts of deionized water; the emulsifier is alkyl alcohol alkoxylated sodium sulfate AS801 and / or sodium vinyl sulfonate; the preparation method of the fluorosilicone polyacrylate emulsion component comprises the following steps: (1) preparing each raw material by weight, then adding an emulsifier and 40% deionized water into a pre-emulsification kettle, then adding an initiator, stirring and mixing evenly, adding an acrylic monomer into the pre-emulsification kettle, and emulsifying for 0.5-1h to obtain a pre-emulsified liquid; (2) Then add the remaining 60% deionized water to the polymerization reactor, stir and heat to 80°C, start to drop the pre-emulsion, control the dropping time to 3.5-4h, after the dropping is completed, heat to 90°C, keep the temperature for reaction for 1h, then cool to 70°C, add fluorine-containing silicon functional monomer, continue to react for 0.5-1.0h, then end the reaction, cool to 30-40°C, adjust the pH value to 7-8 with ammonia water, then add tert-butyl hydroperoxide and Rongalite in sequence to remove the residual acrylic acid monomer in the system, finally add a wetting agent and a defoaming agent, filter and remove impurities, and obtain; The acrylic monomer is glycidyl methacrylate, and one or more of acrylic acid, methyl methacrylate, butyl acrylate, hydroxybutyl acrylate, and hydroxyethyl acrylate; the fluorine-containing silicon functional monomer includes octafluoropentanoic acid and / or perfluorooctanoic acid.

2. The one-component waterproof coating based on fluorosilicone polyacrylate emulsion according to claim 1, characterized in that: The filler component is a combination of 400 mesh heavy calcium, 400 mesh quartz sand, and 400 mesh polytetrafluoroethylene plastic powder; the dispersant is polycarboxylate dispersing water reducer 5040; the defoamer is a mineral oil defoamer and / or a silicone defoamer; the thickener is one of thickeners ASE60 or L344; the dye paste is one of phthalocyanine blue, iron red, chrome yellow, and carbon black paste.

3. A method for preparing a one-component waterproof coating based on fluorosilicone polyacrylate emulsion according to any one of claims 1 to 2, characterized in that: The method comprises the following preparation steps: firstly, the filler component is mixed with deionized water, and a dispersant and a defoamer are added in sequence during the stirring process. After the mixture is evenly stirred, a fluorosilicone polyacrylate emulsion component is added, and the mixture is stirred for 10 minutes. Then, a bactericide and a mildew preventer are added, and then a thickener is added to adjust the viscosity of the system. Finally, a dye paste is added, and the mixture is stirred for 20 minutes to obtain a single-component waterproof coating.

4. An application of a one-component waterproof coating based on fluorosilicone polyacrylate emulsion according to any one of claims 1 to 2, characterized in that: Used in the field of waterproofing and protection of building materials.

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