阅读说明：本技术 一种高抗菌建筑装饰涂料及其制备方法 (High-antibacterial building decorative coating and preparation method thereof ) 是由 代群 代琴 张亮 刘文秀 于 2020-08-03 设计创作，主要内容包括：本发明公开了一种高抗菌建筑装饰涂料及其制备方法,该涂料由如下重量份原料制成：丙烯酸乳液80-100份、三硬脂酸甘油酯1-1.5份、聚二甲基硅氧烷0.5-0.8份、滑石粉12-15份、高岭土粉7-10份、云母粉7-10份、抗菌填料2-3份；将中间体4与改性纳米二氧化钛进行反应,中间体4的结构中含有醛基,醛基在对甲苯磺酸的作用下与改性纳米二氧化钛表面的羟基进行缩合,进而使得中间体4牢牢的固定在改性纳米二氧化钛表面,中间体4含有与苯并咪唑相同的结构,使得制得抗菌填料具有很好的杀菌性,同时与传统有机抗菌剂不同,该抗菌剂不会因涂料长时间使用后从涂料表面析出,进而增加了涂料抗菌效果的耐久性。(The invention discloses a high-antibacterial architectural decorative coating and a preparation method thereof, wherein the coating is prepared from the following raw materials in parts by weight: 80-100 parts of acrylic emulsion, 1-1.5 parts of glyceryl tristearate, 0.5-0.8 part of polydimethylsiloxane, 12-15 parts of talcum powder, 7-10 parts of kaolin powder, 7-10 parts of mica powder and 2-3 parts of antibacterial filler; the intermediate 4 is reacted with the modified nano titanium dioxide, the structure of the intermediate 4 contains aldehyde groups, the aldehyde groups are condensed with hydroxyl groups on the surface of the modified nano titanium dioxide under the action of p-toluenesulfonic acid, so that the intermediate 4 is firmly fixed on the surface of the modified nano titanium dioxide, the intermediate 4 contains a structure the same as benzimidazole, the prepared antibacterial filler has good bactericidal performance, and meanwhile, different from the traditional organic antibacterial agent, the antibacterial agent cannot be separated out from the surface of the coating after the coating is used for a long time, so that the durability of the antibacterial effect of the coating is improved.)

1. A high antibacterial architectural decoration coating is characterized in that: the feed is prepared from the following raw materials in parts by weight: 80-100 parts of acrylic emulsion, 1-1.5 parts of glyceryl tristearate, 0.5-0.8 part of polydimethylsiloxane, 12-15 parts of talcum powder, 7-10 parts of kaolin powder, 7-10 parts of mica powder and 2-3 parts of antibacterial filler;

the decorative coating is prepared by the following steps:

step S1: adding talcum powder, kaolin powder and mica powder into a pulverizer to be pulverized, and mixing after passing through a 1250-mesh and 1300-mesh screen to prepare a mixture;

step S2: adding half of the acrylate emulsion, the mixture prepared in the step S1 and the tristearin into a reaction kettle, stirring for 20-30min under the condition of 800-1000r/min, adding the other half of the acrylate emulsion and the antibacterial filler, and stirring for 10-15min to prepare a mixed base solution;

step S3: and (4) adding the mixed base solution prepared in the step S2 and polydimethylsiloxane into a reaction kettle, and stirring for 30-50min under the condition that the rotating speed is 2000-3000r/min to prepare the waterproof coating.

2. The highly antibacterial architectural decorative coating according to claim 1, wherein: the antibacterial filler is prepared by the following steps:

step A1: adding ethanol into a reaction kettle, stirring and adding n-butyl titanate until the mixed solution becomes transparent under the conditions that the rotation speed is 200-plus-300 r/min and the temperature is 25-30 ℃ to prepare a first mixed solution, adding deionized water and a nitric acid solution into the reaction kettle until the pH value is 3.5-4, stirring and adding the first mixed solution under the condition that the rotation speed is 100-plus-200 r/min to react for 1-1.5h to prepare gel, drying the gel under the condition that the temperature is 70-80 ℃, and roasting for 2-3h under the condition that the temperature is 700-plus-800 ℃ to prepare the nano titanium dioxide;

step A2: adding vinyltriethoxysilane and ethanol into a reaction kettle, stirring until the mixture is uniformly mixed, adding the nano titanium dioxide prepared in the step A1, reacting for 1-2h at the temperature of 100-110 ℃, filtering to remove filtrate, and drying to obtain modified nano titanium dioxide;

step A3: adding p-methylacetanilide, mixed acid and acetic anhydride into a reaction kettle, reacting for 2-3h at the rotation speed of 200-300r/min and the temperature of 25-30 ℃, adding a sulfuric acid solution, and performing reflux reaction for 20-30min at the temperature of 115-120 ℃ to obtain an intermediate 1;

step A4: adding the intermediate 1 and the sodium sulfide solution prepared in the step A3 into a reaction kettle, reacting for 3-4h at the temperature of 120-130 ℃ to prepare an intermediate 2, adding the intermediate 2 and formic acid into the reaction kettle, reacting for 2-3h at the rotation speed of 200-300r/min and the temperature of 100-105 ℃, adding a sodium hydroxide solution until the pH value is 7, and filtering to obtain an intermediate 3;

step A5: adding the intermediate 3 prepared in the step A4 and liquid bromine into a reaction kettle, reacting for 30-40min under the illumination condition of the rotation speed of 100-150r/min, adding a sodium hydroxide solution, reacting for 2-3h under the temperature of 80-90 ℃, adding sodium dodecyl benzene sulfonate and a nitric acid solution under the rotation speed of 200-300r/min and the temperature of 100-105 ℃, and reacting for 3-5h to prepare an intermediate 4;

step A6: and B, adding the intermediate 4 prepared in the step A5 and ethanol into a stirring kettle, stirring until the intermediate 4 is completely dissolved, adding modified nano titanium dioxide and p-toluenesulfonic acid, reacting for 2-3h at the rotation speed of 200-300r/min and the temperature of 40-50 ℃, and distilling to remove the ethanol at the temperature of 80-85 ℃ to prepare the antibacterial filler.

3. The highly antibacterial architectural decorative coating according to claim 2, wherein: the dosage of the ethanol and the butyl titanate in the step A1 is 9:1, the dosage of the deionized water and the ethanol is 1:3 by volume, and the mass fraction of the nitric acid solution is 40-45%.

4. The highly antibacterial architectural decorative coating according to claim 2, wherein: the dosage of the vinyltriethoxysilane in the step A2 is 2.5-3% of the mass of the nano titanium dioxide.

5. The highly antibacterial architectural decorative coating according to claim 2, wherein: the usage ratio of the p-methylacetanilide, the mixed acid, the acetic anhydride and the sulfuric acid solution in the step A3 is 10g:5mL:1mL:2mL, the mixed acid is prepared by mixing concentrated nitric acid and concentrated sulfuric acid in a volume ratio of 2:3, the mass fraction of the concentrated nitric acid is 70-75%, the mass fraction of the concentrated sulfuric acid is 75-80%, and the mass fraction of the sulfuric acid solution is 20-30%.

6. The highly antibacterial architectural decorative coating according to claim 2, wherein: the using amount ratio of the intermediate 1 to the sodium sulfide solution in the step A4 is 5g:2mL, the mass fraction of the sodium sulfide solution is 25-30%, the using amount ratio of the intermediate 2 to formic acid is 2:1, and the mass fraction of the sodium hydroxide solution is 40-45%.

7. The highly antibacterial architectural decorative coating according to claim 2, wherein: the intermediate 3, the liquid bromine, the sodium hydroxide solution, the sodium dodecyl benzene sulfonate and the nitric acid solution are 10g, 3mL, 5mL, 0.02g and 8mL in the step A5, and the mass fraction of the nitric acid solution is 50-55%.

8. The highly antibacterial architectural decorative coating according to claim 2, wherein: the mass ratio of the intermediate 4 to the modified nano titanium dioxide in the step A6 is 1:2, and the mass of the p-toluenesulfonic acid is 2.5-3% of the total mass of the intermediate 4 and the modified nano titanium dioxide.

9. The preparation method of the highly antibacterial architectural decorative coating according to claim 1, characterized in that: the method specifically comprises the following steps:

step S1: adding talcum powder, kaolin powder and mica powder into a pulverizer to be pulverized, and mixing after passing through a 1250-mesh and 1300-mesh screen to prepare a mixture;

step S2: adding half of the acrylate emulsion, the mixture prepared in the step S1 and the tristearin into a reaction kettle, stirring for 20-30min under the condition of 800-1000r/min, adding the other half of the acrylate emulsion and the antibacterial filler, and stirring for 10-15min to prepare a mixed base solution;

step S3: and (4) adding the mixed base solution prepared in the step S2 and polydimethylsiloxane into a reaction kettle, and stirring for 30-50min under the condition that the rotating speed is 2000-3000r/min to prepare the waterproof coating.

Technical Field

The invention belongs to the technical field of paint preparation, and particularly relates to a high-antibacterial building decorative paint and a preparation method thereof.

Background

With the increasing variety of coating products and the continuous expansion of application range, the coating industry has become an important independent industrial production part in the chemical industry, and in the coating industry, powder coating is widely applied to multiple fields of household appliances, indoor and outdoor components, traffic transportation and the like as the powder coating is a new material industry and has the advantages of no organic solvent, excellent physical and mechanical properties, safe production and construction, better chemical resistance and weather resistance, recyclable overspray powder, easy realization of automation of coating, excellent coating performance and the like.

The antibacterial agent can be added into the existing decorative coating in the preparation process in order to improve the antibacterial property of the coating, but although the existing organic antibacterial agent has a good antibacterial effect, the antibacterial component in the coating can be separated out after the coating is used for a period of time, so that the antibacterial effect of the coating is greatly reduced.

Disclosure of Invention

The invention aims to provide a high-antibacterial building decorative coating and a preparation method thereof.

The technical problems to be solved by the invention are as follows:

the antibacterial agent can be added into the existing decorative coating in the preparation process in order to improve the antibacterial property of the coating, but although the existing organic antibacterial agent has a good antibacterial effect, the antibacterial component in the coating can be separated out after the coating is used for a period of time, so that the antibacterial effect of the coating is greatly reduced.

The purpose of the invention can be realized by the following technical scheme:

a high-antibacterial architectural decoration paint is prepared from the following raw materials in parts by weight: 80-100 parts of acrylic emulsion, 1-1.5 parts of glyceryl tristearate, 0.5-0.8 part of polydimethylsiloxane, 12-15 parts of talcum powder, 7-10 parts of kaolin powder, 7-10 parts of mica powder and 2-3 parts of antibacterial filler;

the decorative coating is prepared by the following steps:

step S1: adding talcum powder, kaolin powder and mica powder into a pulverizer to be pulverized, and mixing after passing through a 1250-mesh and 1300-mesh screen to prepare a mixture;

step S2: adding half of the acrylate emulsion, the mixture prepared in the step S1 and the tristearin into a reaction kettle, stirring for 20-30min under the condition of 800-1000r/min, adding the other half of the acrylate emulsion and the antibacterial filler, and stirring for 10-15min to prepare a mixed base solution;

step S3: and (4) adding the mixed base solution prepared in the step S2 and polydimethylsiloxane into a reaction kettle, and stirring for 30-50min under the condition that the rotating speed is 2000-3000r/min to prepare the waterproof coating.

Further, the antibacterial filler is prepared by the following steps:

step A1: adding ethanol into a reaction kettle, stirring and adding n-butyl titanate until the mixed solution becomes transparent under the conditions that the rotation speed is 200-plus-300 r/min and the temperature is 25-30 ℃ to prepare a first mixed solution, adding deionized water and a nitric acid solution into the reaction kettle until the pH value is 3.5-4, stirring and adding the first mixed solution under the condition that the rotation speed is 100-plus-200 r/min to react for 1-1.5h to prepare gel, drying the gel under the condition that the temperature is 70-80 ℃, and roasting for 2-3h under the condition that the temperature is 700-plus-800 ℃ to prepare the nano titanium dioxide;

step A2: adding vinyltriethoxysilane and ethanol into a reaction kettle, stirring until the mixture is uniformly mixed, adding the nano titanium dioxide prepared in the step A1, reacting for 1-2h at the temperature of 100-110 ℃, filtering to remove filtrate, and drying to obtain modified nano titanium dioxide;

step A3: adding p-methylacetanilide, mixed acid and acetic anhydride into a reaction kettle, reacting for 2-3h at the rotation speed of 200-300r/min and the temperature of 25-30 ℃, adding a sulfuric acid solution, and performing reflux reaction for 20-30min at the temperature of 115-120 ℃ to obtain an intermediate 1;

the reaction process is as follows:

step A4: adding the intermediate 1 and the sodium sulfide solution prepared in the step A3 into a reaction kettle, reacting for 3-4h at the temperature of 120-130 ℃ to prepare an intermediate 2, adding the intermediate 2 and formic acid into the reaction kettle, reacting for 2-3h at the rotation speed of 200-300r/min and the temperature of 100-105 ℃, adding a sodium hydroxide solution until the pH value is 7, and filtering to obtain an intermediate 3;

the reaction process is as follows:

step A5: adding the intermediate 3 prepared in the step A4 and liquid bromine into a reaction kettle, reacting for 30-40min under the illumination condition of the rotation speed of 100-150r/min, adding a sodium hydroxide solution, reacting for 2-3h under the temperature of 80-90 ℃, adding sodium dodecyl benzene sulfonate and a nitric acid solution under the rotation speed of 200-300r/min and the temperature of 100-105 ℃, and reacting for 3-5h to prepare an intermediate 4;

the reaction process is as follows:

step A6: and B, adding the intermediate 4 prepared in the step A5 and ethanol into a stirring kettle, stirring until the intermediate 4 is completely dissolved, adding modified nano titanium dioxide and p-toluenesulfonic acid, reacting for 2-3h at the rotation speed of 200-300r/min and the temperature of 40-50 ℃, and distilling to remove the ethanol at the temperature of 80-85 ℃ to prepare the antibacterial filler.

Further, the mass ratio of the ethanol to the butyl titanate in the step A1 is 9:1, the volume ratio of the deionized water to the ethanol is 1:3, and the mass fraction of the nitric acid solution is 40-45%.

Further, the dosage of the vinyltriethoxysilane in the step A2 is 2.5-3% of the mass of the nano titanium dioxide.

Further, the usage ratio of the p-methylacetanilide, the mixed acid, the acetic anhydride and the sulfuric acid solution in the step A3 is 10g:5mL:1mL:2mL, the mixed acid is formed by mixing concentrated nitric acid and concentrated sulfuric acid in a volume ratio of 2:3, the mass fraction of the concentrated nitric acid is 70-75%, the mass fraction of the concentrated sulfuric acid is 75-80%, and the mass fraction of the sulfuric acid solution is 20-30%.

Further, the using amount ratio of the intermediate 1 and the sodium sulfide solution in the step A4 is 5g:2mL, the mass fraction of the sodium sulfide solution is 25-30%, the using amount ratio of the intermediate 2 and formic acid is 2:1, and the mass fraction of the sodium hydroxide solution is 40-45%.

Further, the intermediate 3, the liquid bromine, the sodium hydroxide solution, the sodium dodecyl benzene sulfonate and the nitric acid solution are 10g, 3mL, 5mL, 0.02g and 8mL in the step A5, and the mass fraction of the nitric acid solution is 50-55%.

Further, the mass ratio of the intermediate 4 to the modified nano titanium dioxide in the step A6 is 1:2, and the mass of the p-toluenesulfonic acid is 2.5-3% of the total mass of the intermediate 4 and the modified nano titanium dioxide.

Further, a preparation method of the high-antibacterial architectural decorative coating specifically comprises the following steps:

step S1: adding talcum powder, kaolin powder and mica powder into a pulverizer to be pulverized, and mixing after passing through a 1250-mesh and 1300-mesh screen to prepare a mixture;

step S2: adding half of the acrylate emulsion, the mixture prepared in the step S1 and the tristearin into a reaction kettle, stirring for 20-30min under the condition of 800-1000r/min, adding the other half of the acrylate emulsion and the antibacterial filler, and stirring for 10-15min to prepare a mixed base solution;

step S3: and (4) adding the mixed base solution prepared in the step S2 and polydimethylsiloxane into a reaction kettle, and stirring for 30-50min under the condition that the rotating speed is 2000-3000r/min to prepare the waterproof coating.

The invention has the beneficial effects that: the invention prepares an antibacterial filler in the process of preparing a high-antibacterial building decorative coating, the antibacterial filler takes n-butyl titanate as a raw material to prepare nano titanium dioxide, vinyltriethoxysilane is hydrolyzed to form silanol, the silanol reacts with hydroxyl on the surface of the nano titanium dioxide to form hydrogen bond and is condensed into covalent bond, the silanol is mutually associated and oligomerized to form a film with a net structure, the film is covered on the surface of the nano titanium dioxide, the hydroxyl content on the surface of the titanium dioxide is greatly improved, an intermediate 4 is reacted with the modified nano titanium dioxide, the structure of the intermediate 4 contains aldehyde groups, the aldehyde groups are condensed with the hydroxyl on the surface of the modified nano titanium dioxide under the action of p-toluenesulfonic acid, the intermediate 4 is further firmly fixed on the surface of the modified nano titanium dioxide, the intermediate 4 contains the same structure as benzimidazole, the prepared antibacterial filler has good bactericidal property, and meanwhile, different from the traditional organic antibacterial agent, the antibacterial agent cannot be separated out from the surface of the coating after the coating is used for a long time, so that the durability of the antibacterial effect of the coating is improved.

Detailed Description

The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all 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.