Waterproof primer and preparation method thereof

文档序号：237143 发布日期：2021-11-12 浏览：29次中文

阅读说明：本技术 防水底漆及其制备方法 (Waterproof primer and preparation method thereof ) 是由孙琦汪志勇于 2021-08-16 设计创作，主要内容包括：本发明公开一种防水底漆及其制备方法,涉及涂料技术领域。所述防水底漆包括以下原料：水、羟乙基纤维素、水性添加剂、防霉剂、填料、防冻剂,其中,所述防霉剂包括含氟季铵盐。防水底漆中添加防霉剂,防霉剂包括含氟季铵盐,提高了防霉抗菌效果,另外氟化物具有较好的疏水、耐腐蚀性能,季铵盐中引入了氟,提高了防水涂膜底漆耐碱腐蚀的能力。原子体积较大的氟原子能有效阻挡溶剂的接触,从而提高耐腐蚀的能力,可以有效防止水泥碱性对涂料的侵蚀。(The invention discloses a waterproof primer and a preparation method thereof, and relates to the technical field of coatings. The waterproof primer comprises the following raw materials: the water-based anti-mildew agent comprises water, hydroxyethyl cellulose, a water-based additive, a mildew preventive, a filler and an antifreezing agent, wherein the mildew preventive comprises a fluorine-containing quaternary ammonium salt. The mildew preventive is added into the waterproof primer, the mildew preventive comprises fluorine-containing quaternary ammonium salt, the mildew-proof and antibacterial effects are improved, in addition, fluoride has better hydrophobic and corrosion-resistant properties, and fluorine is introduced into the quaternary ammonium salt, so that the alkali corrosion resistance of the waterproof coating primer is improved. Fluorine atoms with larger atomic volume can effectively block the contact of a solvent, thereby improving the corrosion resistance and effectively preventing the corrosion of the alkalinity of cement to the coating.)

1. The waterproof primer is characterized by comprising the following raw materials:

the water-based anti-mildew agent comprises water, hydroxyethyl cellulose, a water-based additive, a mildew preventive, a filler and an antifreezing agent, wherein the mildew preventive comprises a fluorine-containing quaternary ammonium salt.

2. The water resistant primer of claim 1, wherein the aqueous additive comprises an aqueous dispersant, an aqueous wetting agent, and an aqueous defoamer; and/or the presence of a gas in the gas,

the filler comprises titanium dioxide, mica powder, talcum powder and calcium carbonate; and/or the presence of a gas in the gas,

the antifreeze agent comprises propylene glycol or ethylene glycol.

3. The waterproof primer according to claim 1, wherein the aqueous additive comprises an aqueous dispersant, an aqueous wetting agent and an aqueous defoaming agent, and the mass ratio of the aqueous dispersant to the aqueous wetting agent to the aqueous defoaming agent is 2:1: (1.2-1.5); and/or the presence of a gas in the gas,

the filler comprises titanium dioxide, mica powder, talcum powder and calcium carbonate, and the mass ratio of the titanium dioxide to the mica powder to the talcum powder to the calcium carbonate is (1: 1): (0.8-1): (3-4).

4. The waterproof primer according to claim 1, wherein the waterproof primer comprises the following components in parts by mass:

10-35 parts of water, 0.5-0.6 part of hydroxyethyl cellulose, 4-6 parts of a water-based additive, 0.2-0.3 part of a mildew inhibitor, 50-60 parts of a filler and 0.8-1 part of an antifreezing agent.

5. A method for preparing the waterproof primer according to any one of claims 1 to 4, comprising the steps of:

s10, mixing and stirring water and hydroxyethyl cellulose for 1-3 min, then sequentially adding the water-based additive, the mildew preventive and the filler, and continuously stirring for 15-20 min to obtain a mixture;

and S20, adding an antifreezing agent into the mixture, and stirring and dispersing for 15-20 min to obtain the waterproof primer.

6. The method of preparing a waterproof primer according to claim 5, wherein the method of preparing a waterproof primer further comprises, before step S10:

s101, mixing chitosan, water and isopropanol, stirring at 0-30 ℃, adding a fluorine-containing quaternary ammonium salt and sodium hydroxide, heating to 55-85 ℃, and reacting to obtain a solid A;

s102, mixing the solid A with N, N-dimethylformamide, adding isopropanol and epoxy chloropropane, adjusting the pH value to 7-8, and reacting to obtain a solid B;

s103, mixing the solid B with dimethyl sulfoxide, stirring at 55-85 ℃, adding a beta-cyclodextrin solution, and reacting at constant temperature to obtain the mildew preventive.

7. The method of preparing a waterproof primer according to claim 6, further comprising, before step S101:

s100, mixing perfluorohexylethyl iodide, N-methyldiethanolamine and a solvent uniformly, and stirring at 70-90 ℃ for reaction to obtain the fluorine-containing quaternary ammonium salt.

8. The method for preparing a waterproof primer according to claim 7, wherein the solvent comprises n-butanol; and/or the presence of a gas in the gas,

the mol ratio of the perfluorohexylethyl iodide to the N-methyldiethanolamine is 1: (1-2.5); and/or the presence of a gas in the gas,

the volume of the solvent added into each gram of N-methyldiethanolamine is 10-30 mL.

9. The method for preparing the waterproof primer according to claim 6, wherein in step S102, the volumes of N, N-dimethylformamide, isopropanol and epichlorohydrin added to each gram of the solid A are 20-30 mL, 5-10 mL and 8-20 mL respectively.

10. The method for preparing the waterproof primer according to claim 6, wherein in step S103, the volumes of the dimethyl sulfoxide and the β -cyclodextrin solution added to each gram of the solid B are 20 to 40mL and 20 to 50mL in sequence.

Technical Field

The invention relates to the technical field of coatings, and particularly relates to a waterproof primer and a preparation method thereof.

Background

The building exterior wall base material is mostly cement mortar or concrete surface, and is characterized in that the building exterior wall base material is provided with multiple gaps and strong alkalinity, wherein the porous structure ensures strong water absorption, alkali bloom is generated after soaking in moisture, water and the like, the condition causes crater-shaped bulges to be formed on the surface of a paint film, a layer of alkali cream is formed on the surface of the paint film when the crater-shaped bulges are serious, the paint film is damaged, the surface of the paint film is not smooth enough, the paint film is easy to wrinkle, and the paint film is possibly dried too fast to cause the cracking of the finish paint and waste the finish paint; the strong alkalinity can cause chemical degradation of resin in the coating, accelerate the aging of the coating film and reduce the service life of the coating.

The coating of a layer of sealing primer before the finish paint is coated can save the decoration cost, and the coating of the primer has the advantage of twice the result of the half effort in the long term and the decoration effect; the primer used on the wall surface mainly plays a role in sealing, so that the corrosion of the alkalinity of cement to the paint is prevented; meanwhile, the wall surface is smoother due to the good adhesive force of the primer, the finish paint is easier to brush, and the using amount of the finish paint is reduced.

However, the existing primer has poor alkali corrosion resistance after being brushed and is easy to lose efficacy.

Disclosure of Invention

The invention mainly aims to provide a waterproof primer and a preparation method thereof, and aims to provide an alkali-resistant and corrosion-resistant waterproof primer.

In order to achieve the purpose, the invention provides a waterproof primer which comprises the following raw materials:

Optionally, the aqueous additive comprises an aqueous dispersant, an aqueous wetting agent, and an aqueous defoamer; and/or the presence of a gas in the gas,

the filler comprises titanium dioxide, mica powder, talcum powder and calcium carbonate; and/or the presence of a gas in the gas,

the antifreeze agent comprises propylene glycol or ethylene glycol.

Optionally, the aqueous additive comprises an aqueous dispersing agent, an aqueous wetting agent and an aqueous defoaming agent, and the mass ratio of the aqueous dispersing agent to the aqueous wetting agent to the aqueous defoaming agent is 2:1: (1.2-1.5); and/or the presence of a gas in the gas,

Optionally, the waterproof primer comprises the following components in parts by weight:

10-35 parts of water, 0.5-0.6 part of hydroxyethyl cellulose, 4-6 parts of a water-based additive, 0.2-0.3 part of a mildew inhibitor, 50-60 parts of a filler and 0.8-1 part of an antifreezing agent.

The invention further provides a preparation method of the waterproof primer, which comprises the following steps:

and S20, adding an antifreezing agent into the mixture, and stirring and dispersing for 15-20 min to obtain the waterproof primer.

Optionally, before step S10, the method for preparing the waterproof primer further includes:

s101, mixing chitosan, water and isopropanol, stirring at 0-30 ℃, adding a fluorine-containing quaternary ammonium salt and sodium hydroxide, heating to 55-85 ℃, and reacting to obtain a solid A;

s102, mixing the solid A with N, N-dimethylformamide, adding isopropanol and epoxy chloropropane, adjusting the pH value to 7-8, and reacting to obtain a solid B;

s103, mixing the solid B with dimethyl sulfoxide, stirring at 55-85 ℃, adding a beta-cyclodextrin solution, and reacting at constant temperature to obtain the mildew preventive.

Optionally, before step S101, the method further includes:

s100, mixing perfluorohexylethyl iodide, N-methyldiethanolamine and a solvent uniformly, and stirring at 70-90 ℃ for reaction to obtain the fluorine-containing quaternary ammonium salt.

Optionally, the solvent comprises n-butanol; and/or the presence of a gas in the gas,

the mol ratio of the perfluorohexylethyl iodide to the N-methyldiethanolamine is 1: (1-2.5); and/or the presence of a gas in the gas,

the volume of the solvent added into each gram of N-methyldiethanolamine is 10-30 mL.

Optionally, in step S102, the volumes of N, N-dimethylformamide, isopropanol and epichlorohydrin added to each gram of the solid a are 20 to 30mL, 5 to 10mL and 8 to 20mL in sequence.

Optionally, in step S103, the volumes of the dimethyl sulfoxide and the β -cyclodextrin solution correspondingly added to each gram of the solid B are 20 to 40mL and 20 to 50mL in sequence.

In the technical scheme of the invention, the waterproof primer is provided and comprises the following raw materials: the water-based anti-mildew agent comprises water, hydroxyethyl cellulose, a water-based additive, a mildew preventive, a filler and an antifreezing agent, wherein the mildew preventive comprises a fluorine-containing quaternary ammonium salt. The waterproof primer can form a waterproof coating on a cement base surface, water and water vapor are effectively blocked, the mildew preventive is added into the waterproof primer, the mildew preventive comprises fluorine-containing quaternary ammonium salt, the mildew-proof antibacterial effect is improved, in addition, fluoride has better hydrophobic and corrosion-resistant properties, fluorine is introduced into the quaternary ammonium salt, and the alkali corrosion resistance of the waterproof coating primer is improved. Fluorine atoms with larger atomic volume can effectively block the contact of a solvent, thereby improving the corrosion resistance and effectively preventing the corrosion of the alkalinity of cement to the coating.

Drawings

In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the structures shown in the drawings without creative efforts.

Fig. 1 is a schematic flow chart of an embodiment of a method for preparing a waterproof primer according to the present invention.

The implementation, functional features and advantages of the objects of the present invention will be further explained with reference to the accompanying drawings.

Detailed Description

The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.

It should be noted that, if directional indications (such as upper, lower, left, right, front, rear, outer and inner … …) are involved in the embodiment of the present invention, the directional indications are only used to explain the relative position relationship between the components, the motion situation, etc. in a specific posture (as shown in the drawing), and if the specific posture is changed, the directional indications are changed accordingly.

In addition, if there is a description of "first", "second", etc. in an embodiment of the present invention, the description of "first", "second", etc. is for descriptive purposes only and is not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include at least one such feature. In addition, the meaning of "and/or" appearing throughout includes three juxtapositions, exemplified by "A and/or B" including either A or B or both A and B. In addition, technical solutions between various embodiments may be combined with each other, but must be realized by a person skilled in the art, and when the technical solutions are contradictory or cannot be realized, such a combination should not be considered to exist, and is not within the protection scope of the present invention.

The existing primer has poor alkali corrosion resistance and is easy to lose efficacy after being brushed.

In view of this, the present invention provides a waterproof primer, and aims to provide an alkali-resistant and corrosion-resistant waterproof primer. In the attached drawings, fig. 1 is a schematic flow chart of an embodiment of a preparation method of a waterproof primer provided by the invention.

The invention provides a waterproof primer, which comprises the following raw materials: the water-based anti-mildew agent comprises water, hydroxyethyl cellulose, a water-based additive, a mildew preventive, a filler and an antifreezing agent, wherein the mildew preventive comprises a fluorine-containing quaternary ammonium salt.

The hydroxyethyl cellulose is prepared by etherification reaction of alkali cellulose and ethylene oxide (or chloroethanol), has the characteristics of good thickening, suspension, dispersion, emulsification, adhesion, film formation, moisture protection, protective colloid supply and the like, and can ensure the stability and uniformity of film formation.

The addition of the aqueous additive mainly plays roles of dispersing, wetting, defoaming and the like, preferably, the aqueous additive comprises an aqueous dispersant, an aqueous wetting agent and an aqueous defoaming agent, the invention is not limited by the proportion of the components, and preferably, the mass ratio of the aqueous dispersant to the aqueous wetting agent to the aqueous defoaming agent is 2:1: (1.2 to 1.5), for example, 2:1:1.2, 2:1:1.3, 2:1:1.4, 2:1:1.5, etc., and the waterproof primer obtained in the above-mentioned ratio is stable.

Specifically, in the present embodiment, the aqueous dispersant is a sodium polycarboxylate type dispersant; the water-based wetting agent is wetting agent X-405; the water-based defoaming agent is an organic silicon defoaming agent, so that the compatibility and the stability of the waterproof primer are good.

Preferably, in the embodiment of the invention, the mildew inhibitor not only comprises the fluorine-containing quaternary ammonium salt, but also comprises beta-cyclodextrin and chitosan, and the beta-cyclodextrin is used for loading the chitosan and the fluorine-containing quaternary ammonium salt, so that the stability of the active ingredients in the waterproof primer can be ensured.

The invention is not limited to the type of the filler, preferably, the filler comprises titanium dioxide, mica powder, talcum powder and calcium carbonate, and the mass ratio of the titanium dioxide to the mica powder to the talcum powder to the calcium carbonate is preferably 1: (0.8-1): (3-4), the processing performance of the waterproof primer is improved and the cost is reduced under the above proportion.

The addition of the antifreezing agent can prevent the water in each raw material in the waterproof primer from freezing at low temperature, and the type of the antifreezing agent is not limited in the invention.

The invention is not limited to the proportion of each component in the waterproof primer, and preferably, the waterproof primer comprises the following components in parts by weight: 10-35 parts of water, 0.5-0.6 part of hydroxyethyl cellulose, 4-6 parts of a water-based additive, 0.2-0.3 part of a mildew inhibitor, 50-60 parts of a filler and 0.8-1 part of an antifreezing agent. The waterproof primer has the best alkali resistance, corrosion resistance and waterproofness under the above proportion.

Referring to fig. 1, the present invention further provides a method for preparing the waterproof primer, which comprises the following steps:

and S20, adding an antifreezing agent into the mixture, and stirring and dispersing for 15-20 min to obtain the waterproof primer.

Preferably, in the embodiment of the present invention, the mildew inhibitor is prepared by itself, and before step S10, the method for preparing the waterproof primer further includes:

s11, preparing the mildew preventive containing the fluorine-containing quaternary ammonium salt.

Specifically, step S11 includes:

s101, mixing chitosan, water and isopropanol, stirring at 0-30 ℃, adding a fluorine-containing quaternary ammonium salt and sodium hydroxide, heating to 55-85 ℃, and reacting to obtain a solid A;

in the step, chitosan and fluorine-containing quaternary ammonium salt are compounded, preferably, the mass ratio of the chitosan to the water to the isopropanol to the quaternary ammonium salt to the sodium hydroxide is 2: (10-30): (10-30): 7: in the above-mentioned ratio, the unit of mass is g and the unit of volume is mL, and the combination of both of the solid A and the solid A is preferable in the above-mentioned ratio.

Specifically, the fluorine-containing quaternary ammonium salt is prepared by the following steps:

s100, mixing perfluorohexylethyl iodide, N-methyldiethanolamine and a solvent uniformly, and stirring at 70-90 ℃ for reaction to obtain the fluorine-containing quaternary ammonium salt.

The present invention does not limit the kind of the solvent in step S100, and preferably, the solvent includes n-butanol, which has a good dispersing effect.

The invention also does not limit the mixture ratio of the components, and preferably, the mol ratio of the perfluorohexylethyl iodide to the N-methyldiethanolamine is 1: (1-2.5), the volume of the solvent added into each gram of N-methyldiethanolamine is 10-30 mL, and the obtained fluorine-containing quaternary ammonium salt is good in uniformity and stability under the above proportioning.

S102, mixing the solid A with N, N-dimethylformamide, adding isopropanol and epoxy chloropropane, adjusting the pH value to 7-8, and reacting to obtain a solid B;

activating the surface of the solid A, preferably, the volumes of N, N-dimethylformamide, isopropanol and epichlorohydrin which are correspondingly added to each gram of the solid A are 20-30 mL, 5-10 mL and 8-20 mL in sequence, that is, the ratio of the mass of the solid A, the volume of the N, N-dimethylformamide, the volume of the isopropanol and the volume of the epichlorohydrin is 1: (20-30): (5-10): (8-20), wherein the unit of mass of the solid A is g, and the unit of volume of N, N-dimethylformamide, the unit of volume of isopropanol and the unit of volume of epichlorohydrin are mL, and the solid B has good activation effect under the above proportion.

S103, mixing the solid B with dimethyl sulfoxide, stirring at 55-85 ℃, adding a beta-cyclodextrin solution, and reacting at constant temperature to obtain the mildew preventive.

In this step, the surface of solid B, i.e., chitosan and the fluorine-containing quaternary ammonium salt, is coated with β -cyclodextrin, preferably, the volumes of the dimethyl sulfoxide and the β -cyclodextrin solution added to each gram of solid B are 20 to 40mL and 20 to 50mL in sequence, that is, the ratio of the mass of solid B, the volume of dimethyl sulfoxide and the volume of β -cyclodextrin solution is 1: (20-40): (20-50), in the above proportion, the unit of mass is g, the unit of volume is mL, and the mildew preventive obtained has good mildew-proof effect under the above proportion.

In the examples of the present invention, the beta-cyclodextrin solution used was beta-cyclodextrin and 0.1mol/L sodium hydroxide solution in a ratio of 1 g: 10mL of the above-mentioned components were mixed.

The preparation method of the waterproof primer provided by the invention is simple and convenient, is convenient to operate, has all the beneficial effects of the waterproof primer, and is not repeated herein.

An example of a method for preparing the waterproof primer according to the present invention is given below:

(1) mixing perfluorohexylethyl iodide, N-methyldiethanolamine and a solvent (N-butanol) uniformly, stirring and reacting at 70-90 ℃ for 24 hours, after the reaction is finished, distilling under reduced pressure to remove the solvent, separating and purifying by silica gel column chromatography, and drying under vacuum at 50 ℃ to obtain the fluorine-containing quaternary ammonium salt, wherein the molar ratio of the perfluorohexylethyl iodide to the N-methyldiethanolamine is 1: (1-2.5), the mass ratio of the N-methyldiethanolamine to the volume of the solvent is 1 g: (10-30 mL);

(2) mixing chitosan, water and isopropanol, stirring at 0-30 ℃, adding fluorine-containing quaternary ammonium salt and sodium hydroxide, heating to 55-85 ℃, reacting for 48 hours, cooling, adjusting the pH to 7, treating for 24 hours by using a Soxhlet extractor, and drying at 40 ℃ to constant weight to obtain a solid A;

(3) mixing the solid A with N, N-dimethylformamide, then adding isopropanol and epoxy chloropropane, adjusting the pH value to 7-8, reacting for 10 hours, washing with methanol, and drying at 50 ℃ to constant weight to obtain a solid B, wherein the ratio of the mass of the solid A to the volume of the N, N-dimethylformamide to the volume of the isopropanol to the volume of the epoxy chloropropane is 1 g: (20-30 mL): (5-10 mL): (8-20 mL);

(4) mixing the solid B with dimethyl sulfoxide, stirring for 30min at 55-85 ℃, adding a beta-cyclodextrin solution, reacting for 4h at a constant temperature, performing vacuum filtration, and drying to constant weight at 40 ℃ to obtain the mildew preventive, wherein the ratio of the mass of the solid B to the volume of the dimethyl sulfoxide to the volume of the beta-cyclodextrin solution is 1 g: (20-40 mL): (20-50 mL), wherein the beta-cyclodextrin solution is a mixture of beta-cyclodextrin and 0.1mol/L sodium hydroxide solution according to a ratio of 1 g: 10mL of the mixture is mixed;

(5) mixing 10-35 parts of water and 0.5-0.6 part of hydroxyethyl cellulose for stirring for 1-3 min, sequentially adding 4-6 parts of water-based additive (the mass ratio of the water-based dispersant to the water-based wetting agent to the water-based defoaming agent is 2:1 (1.2-1.5), the water-based dispersant is a sodium polycarboxylate dispersant, the water-based wetting agent is wetting agent X-405, the water-based defoaming agent is an organic silicon defoaming agent), 0.2-0.3 part of mildew preventive and 50-60 parts of filler (the mass ratio of titanium dioxide to mica powder to calcium carbonate is 1:1 (0.8-1) (3-4)), and continuously stirring for 15-20 min to obtain a mixture;

(6) and adding 0.8-1 part of an antifreezing agent (propylene glycol or ethylene glycol) into the mixture, and stirring and dispersing for 15-20 min to obtain the waterproof primer.

The technical solutions of the present invention are further described in detail with reference to the following specific examples, which should be understood as merely illustrative and not limitative.

Example 1

(1) Mixing perfluorohexylethyl iodide, N-methyldiethanolamine and a solvent (N-butanol) uniformly, stirring and reacting at 80 ℃ for 24 hours, after the reaction is finished, distilling under reduced pressure to remove the solvent, separating and purifying by silica gel column chromatography, and drying under vacuum at 50 ℃ to obtain the fluorine-containing quaternary ammonium salt, wherein the molar ratio of the perfluorohexylethyl iodide to the N-methyldiethanolamine is 1: the ratio of the mass of the 1, N-methyldiethanolamine to the volume of the solvent is 1 g: 10 mL;

(2) mixing chitosan, deionized water and isopropanol, stirring at 30 ℃, adding fluorine-containing quaternary ammonium salt and sodium hydroxide, heating to 85 ℃, reacting for 48 hours, cooling, adjusting the pH to 7, treating for 24 hours by using a Soxhlet extractor, and drying at 40 ℃ to constant weight to obtain a solid A, wherein the dosage ratio of the chitosan, the deionized water, the isopropanol, the quaternary ammonium salt and the sodium hydroxide is 2 g: 10mL of: 10mL of: 7 g: 25g of the total weight of the mixture;

(3) mixing the solid A with N, N-dimethylformamide, then adding isopropanol and epoxy chloropropane, adjusting the pH value to 7, reacting for 10 hours, washing with methanol, drying at 50 ℃ to constant weight to obtain a solid B, wherein the ratio of the mass of the solid A, the volume of the N, N-dimethylformamide, the volume of the isopropanol and the volume of the epoxy chloropropane is 1 g: 20mL of: 5mL of: 8 mL;

(4) mixing the solid B with dimethyl sulfoxide, stirring for 30min at 60 ℃, adding a beta-cyclodextrin solution, reacting for 4h at constant temperature, carrying out vacuum filtration, drying to constant weight at 40 ℃ to obtain the mildew preventive, wherein the ratio of the mass of the solid B to the volume of the dimethyl sulfoxide to the volume of the beta-cyclodextrin solution is 1 g: 20mL of: 20mL, the beta-cyclodextrin solution is beta-cyclodextrin and 0.1mol/L sodium hydroxide solution according to the weight ratio of 1 g: 10mL of the mixture is mixed;

(5) mixing 10 parts of water and 0.5 part of hydroxyethyl cellulose, stirring for 1min, sequentially adding 4 parts of water-based additive (the mass ratio of the water-based dispersant to the water-based wetting agent to the water-based defoaming agent is 2:1:1.2, the water-based dispersant is a sodium polycarboxylate type dispersant, the water-based wetting agent is wetting agent X-405, the water-based defoaming agent is an organic silicon defoaming agent), 0.2 part of mildew preventive and 50 parts of filler (the mass ratio of titanium dioxide to mica powder to talcum powder to calcium carbonate is 1: 1: 0.8: 3), and continuously stirring for 15-20 min to obtain a mixture;

(6) and adding 0.8 part of antifreezing agent (propylene glycol) into the mixture, and stirring and dispersing for 15min to obtain the waterproof primer.

Example 2

(5) mixing 20 parts of water and 0.5 part of hydroxyethyl cellulose, stirring for 3min, sequentially adding 5 parts of water-based additive (the mass ratio of the water-based dispersant to the water-based wetting agent to the water-based defoaming agent is 2:1:1.3, the water-based dispersant is a sodium polycarboxylate type dispersant, the water-based wetting agent is wetting agent X-405, the water-based defoaming agent is an organic silicon defoaming agent), 0.3 part of mildew preventive and 55 parts of filler (the mass ratio of titanium dioxide to mica powder to talcum powder to calcium carbonate is 1: 1: 0.9: 3.5), and continuously stirring for 18min to obtain a mixture;

(6) and adding 0.9 part of antifreezing agent (propylene glycol) into the mixture, and stirring and dispersing for 18min to obtain the waterproof primer.

Example 3

(5) mixing 35 parts of water and 0.6 part of hydroxyethyl cellulose, stirring for 3min, sequentially adding 6 parts of water-based additive (the mass ratio of the water-based dispersant to the water-based wetting agent to the water-based defoaming agent is 2:1:1.5, the water-based dispersant is a sodium polycarboxylate type dispersant, the water-based wetting agent is wetting agent X-405, the water-based defoaming agent is an organic silicon defoaming agent), 0.3 part of mildew preventive and 60 parts of filler (the mass ratio of titanium dioxide, mica powder, talcum powder and calcium carbonate is 1: 1: 4), and continuously stirring for 20min to obtain a mixture;

(6) and adding 1 part of an antifreezing agent (ethylene glycol) into the mixture, and stirring and dispersing for 20min to obtain the waterproof primer.

Example 4

(1) Mixing perfluorohexylethyl iodide, N-methyldiethanolamine and a solvent (N-butanol) uniformly, stirring and reacting at 70 ℃ for 24 hours, after the reaction is finished, distilling under reduced pressure to remove the solvent, separating and purifying by silica gel column chromatography, and drying under vacuum at 50 ℃ to obtain the fluorine-containing quaternary ammonium salt, wherein the molar ratio of the perfluorohexylethyl iodide to the N-methyldiethanolamine is 1: 2.5, the ratio of the mass of N-methyldiethanolamine to the volume of the solvent is 1 g: 30 mL;

(2) mixing chitosan, water and isopropanol, stirring at 0 ℃, adding fluorine-containing quaternary ammonium salt and sodium hydroxide, heating to 55 ℃, reacting for 48 hours, cooling, adjusting the pH to 7, treating for 24 hours by using a Soxhlet extractor, and drying at 40 ℃ to constant weight to obtain a solid A, wherein the dosage ratio of the chitosan, the deionized water, the isopropanol, the quaternary ammonium salt and the sodium hydroxide is 2 g: 30mL of: 30mL of: 7 g: 25g of the total weight of the mixture;

(3) mixing the solid A with N, N-dimethylformamide, then adding isopropanol and epoxy chloropropane, adjusting the pH value to 8, reacting for 10 hours, washing with methanol, drying at 50 ℃ to constant weight to obtain a solid B, wherein the ratio of the mass of the solid A, the volume of the N, N-dimethylformamide, the volume of the isopropanol and the volume of the epoxy chloropropane is 1 g: 30mL of: 10mL of: 20 mL;

(4) mixing the solid B with dimethyl sulfoxide, stirring for 30min at 55 ℃, adding a beta-cyclodextrin solution, reacting for 4h at constant temperature, carrying out vacuum filtration, drying to constant weight at 40 ℃ to obtain the mildew preventive, wherein the ratio of the mass of the solid B to the volume of the dimethyl sulfoxide to the volume of the beta-cyclodextrin solution is 1 g: 40mL of: 50mL of beta-cyclodextrin solution is prepared by mixing beta-cyclodextrin and 0.1mol/L of sodium hydroxide solution according to the weight ratio of 1 g: 10mL of the mixture is mixed;

(5) mixing and stirring 22 parts of water and 0.5 part of hydroxyethyl cellulose for 2min, sequentially adding 5 parts of water-based additive (the mass ratio of the water-based dispersant to the water-based wetting agent to the water-based defoaming agent is 2:1:1, 4, the water-based dispersant is a sodium polycarboxylate type dispersant, the water-based wetting agent is wetting agent X-405, the water-based defoaming agent is an organic silicon defoaming agent), 0.2 part of mildew preventive and 58 parts of filler (the mass ratio of titanium dioxide, mica powder, talcum powder and calcium carbonate is 1: 1: 0.8: 4), and continuously stirring for 17min to obtain a mixture;

(6) and adding 0.8 part of antifreezing agent (propylene glycol) into the mixture, and stirring and dispersing for 16min to obtain the waterproof primer.

Example 5

(1) Mixing perfluorohexylethyl iodide, N-methyldiethanolamine and a solvent (N-butanol) uniformly, stirring and reacting at 90 ℃ for 24 hours, after the reaction is finished, distilling under reduced pressure to remove the solvent, separating and purifying by silica gel column chromatography, and drying under vacuum at 50 ℃ to obtain the fluorine-containing quaternary ammonium salt, wherein the molar ratio of the perfluorohexylethyl iodide to the N-methyldiethanolamine is 1: 1.8, the ratio of the mass of N-methyldiethanolamine to the volume of the solvent is 1 g: 20 mL;

(2) mixing chitosan, water and isopropanol, stirring at 15 ℃, adding fluorine-containing quaternary ammonium salt and sodium hydroxide, heating to 70 ℃, reacting for 48 hours, cooling, adjusting the pH to 7, treating for 24 hours by using a Soxhlet extractor, and drying at 40 ℃ to constant weight to obtain a solid A;

(4) mixing the solid B with dimethyl sulfoxide, stirring for 30min at 85 ℃, adding a beta-cyclodextrin solution, reacting for 4h at constant temperature, carrying out vacuum filtration, drying to constant weight at 40 ℃ to obtain the mildew preventive, wherein the ratio of the mass of the solid B to the volume of the dimethyl sulfoxide to the volume of the beta-cyclodextrin solution is 1 g: 30mL of: 35mL, the beta-cyclodextrin solution is beta-cyclodextrin and 0.1mol/L sodium hydroxide solution according to the weight ratio of 1 g: 10mL of the mixture is mixed;

(5) mixing 30 parts of water and 0.6 part of hydroxyethyl cellulose, stirring for 3min, sequentially adding 6 parts of water-based additive (the mass ratio of the water-based dispersant to the water-based wetting agent to the water-based defoaming agent is 2:1:1.5, the water-based dispersant is a sodium polycarboxylate type dispersant, the water-based wetting agent is wetting agent X-405, the water-based defoaming agent is an organic silicon defoaming agent), 0.2 part of mildew preventive and 59 parts of filler (the mass ratio of titanium dioxide, mica powder, talcum powder and calcium carbonate is 1: 1: 3), and continuously stirring for 16min to obtain a mixture;

(6) and adding 1 part of an antifreezing agent (propylene glycol) into the mixture, and stirring and dispersing for 19min to obtain the waterproof primer.

Comparative example 1

The procedure and starting materials were the same as in example 1 except that perfluorohexylethyl iodide in the step (1) was replaced with epichlorohydrin.

Comparative example 2

The procedure and raw materials were the same as in example 1 except that the steps (1) to (4) were omitted and the fungicide in step (5) was replaced with an isothiazolinone fungicide.

The waterproof primers prepared in examples 1 to 5 and comparative examples 1 to 2 were tested using commercially available construction cement and construction yellow sand in a mass ratio of 1: 3, adding a proper amount of water, uniformly stirring, scraping to form a cement mortar surface, respectively and uniformly coating the waterproof primers prepared in the examples 1 to 5 and the comparative examples 1 to 2 on the cement mortar surface after the mortar is dried for 7 days and is dried for 1 month, coating the water-based exterior wall latex paint after drying for 2 days, and performing a water spraying test to test the surface saltpetering of the finish paint after drying for 7 days, wherein the test results are shown in the following table 1.

TABLE 1 examples 1-5 and comparative examples 1-2 Ustilagine conditions

Referring to table 1, it can be seen that the waterproof primers prepared in examples 1 to 5 of the present invention all make the top coat normal and have no saltpetering after being used, while the quaternary ammonium salt used in comparative example 1 does not contain fluorine, and the mildew preventive comprising fluorine-containing quaternary ammonium salt is not used in comparative example 2, and the saltpetering phenomenon occurs, and it is seen that the use of the mildew preventive comprising fluorine-containing quaternary ammonium salt is very important, and the alkali corrosion resistance of the waterproof primer is improved.

In conclusion, the waterproof primer provided by the invention improves the mildew-proof and antibacterial effects, and in addition, the fluoride has better hydrophobic and corrosion-resistant properties, and the fluorine is introduced into the quaternary ammonium salt, so that the alkali corrosion resistance of the waterproof coating primer is improved, the waterproof coating primer can replace the existing primer product, and the waterproof primer can be widely applied to coating products.

The above description is only a preferred embodiment of the present invention, and is not intended to limit the scope of the present invention, and all modifications and equivalents of the present invention, which are made by the contents of the present specification and the accompanying drawings, or directly/indirectly applied to other related technical fields, are included in the scope of the present invention.

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Waterproof primer and preparation method thereof

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