CN115505316A - Anticorrosive clean-keeping nano coating material and preparation method thereof - Google Patents
Anticorrosive clean-keeping nano coating material and preparation method thereof Download PDFInfo
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Abstract
The invention relates to the field of coating materials, and discloses an anticorrosive clean-keeping nano coating material and a preparation method thereof. Stirring and mixing hexamethyldisilazane and ethanol water solution to obtain a mixed solution; mixing nano SiO 2 Adding the mixture into the mixed solution, stirring and mixing the mixture, and drying the mixture in vacuum to obtain modified nano SiO 2 (ii) a Modified nano SiO 2 After the secondary modification of n-octyl triethoxysilane, the secondary modified nano SiO is obtained 2 . Secondary modified nano SiO 2 Not only obviously improves the dispersibility in the oily anticorrosive pigment; meanwhile, the hydrophilic surface rich in hydroxyl is converted into a hydrophobic surface containing organic functional groups, so that the nano SiO is improved 2 Self-cleaning property of (2). The secondary modified nano SiO 2 Mixing the epoxy resin, the fluorocarbon resin and the curing agent to prepare the coating material. Nano SiO 2 2 The synergistic effect of the inorganic filler and the fluorocarbon resin can obviously improve the corrosion resistance of the coating material, so that the prepared nano coating material has the advantages of self-cleaning and high corrosion resistance.
Description
Technical Field
The invention relates to the technical field of nano coating materials, in particular to an anticorrosive clean-keeping nano coating material and a preparation method thereof.
Background
On the surface of a base material such as glass ceramic or wood stone, the coating material has the characteristics of hydrophobicity and high corrosion resistance, and can play the roles of self-cleaning and corrosion resistance. Namely, the coating has chemical corrosion resistance and can reduce the contact area between pollutants such as dust and the like and the surface of the coating when the pollutants are contacted with the surface of the coating, thereby leading the coating to have excellent automatic cleaning performance. The technical research on anticorrosion and self-cleaning performances of coating materials in counties is as follows:
chinese patent application CN110511646A discloses a preparation method of an anticorrosive coating material with a self-cleaning effect. The hydrophobic surface layer of the anticorrosive coating material comprises nano silicon dioxide modified by a silane coupling agent. Chinese patent CN105419633B discloses a preparation process of an anticorrosive self-cleaning coating for bridges. By adding the nano-scale silicon dioxide, the aging resistance and the self-cleaning performance of the coating are enhanced.
However, the above patents are all based on the characteristics of the nano-silica or are only modified by a coupling agent to prepare the anticorrosive self-cleaning coating. However, the nano-silica has many hydrophilic hydroxyl groups, so that the nano-silica has poor dispersibility in the coating and poor corrosion resistance.
Disclosure of Invention
In order to solve the technical problems, the invention provides an antiseptic clean-keeping nano coating material and a preparation method thereof,
in order to realize the aim, the invention discloses a preparation method of an anticorrosive clean-keeping nano coating material, which comprises the following steps:
step one, stirring and mixing hexamethyldisilazane and an ethanol water solution to obtain a mixed solution; mixing nano SiO 2 Adding the mixture into the mixed solution, stirring and mixing the mixture, and drying the mixture in vacuum to obtain modified nano SiO 2 ；
Stirring and mixing n-octyl triethoxysilane and an ethanol water solution to obtain hydrolyzed n-octyl triethoxysilane; adding ammonia water and modified nano-scale into dissolved n-octyl triethoxysilaneSiO 2 Stirring, mixing and ultrasonic dispersing to obtain dispersed SiO 2 A solution;
step three, dispersing the SiO 2 Carrying out water bath reaction on the solution, and centrifuging to obtain a centrifuged product; drying and grinding the centrifuged product to obtain the secondary modified nano SiO 2 Powder;
step four, carrying out secondary modification on the nano SiO 2 The powder, the epoxy resin powder, the fluorocarbon resin powder and the dicyandiamide powder are mixed and dispersed evenly to obtain the anticorrosion clean-keeping nano coating material.
Preferably, in the step one, nano SiO 2 The mass ratio of the hexamethyldisilazane to the ethanol aqueous solution is (80-100) to (10-20) to 100-150.
Preferably, the ethanol water solution is 95% by mass.
Preferably, in the first step, the stirring and mixing conditions are as follows: the stirring and mixing speed is 300-500r/min, and the stirring and mixing time is 1-2h.
Preferably, in the step one, the temperature of vacuum drying is 50-60 ℃, the time of vacuum drying is 300-400min, and the vacuum degree is-0.05 to-0.08 MPa.
Preferably, in the second step, the volume ratio of the n-octyltriethoxysilane to the ethanol aqueous solution is 1.
Preferably, in the second step, the stirring and mixing conditions are as follows: the stirring and mixing speed is 300-500r/min, and the stirring and mixing time is 1-2h; the ultrasonic dispersion conditions are as follows: the ultrasonic frequency is 500W, and the ultrasonic dispersion time is 30-60min.
Preferably, in the second step, the modified nano SiO 2 The mass ratio of the hydrolyzed n-octyl triethoxysilane to the ammonia water is (3-15) to (80);
the ammonia water is prepared by mixing high-concentration ammonia water and deionized water;
the volume ratio of the deionized water to the high-concentration ammonia water is (15-20) to 5;
the concentration of the high-concentration ammonia water is 15-25wt%.
Preferably, in the third step, the temperature of the water bath reaction is 40-45 ℃, the duration of the water bath reaction is 12h, the stirring speed of the water bath reaction is 300-400r/min, and the drying condition is that the drying is carried out for 3-5h at the temperature of 50-70 ℃.
Preferably, in the fourth step, the nano SiO modified twice 2 The mass ratio of the powder, the epoxy resin powder, the fluorocarbon resin powder and the dicyandiamide powder is (10-30): 80, (5-20): 10.
The invention also discloses the anticorrosive clean-keeping nano coating material prepared by the method for preparing the anticorrosive clean-keeping nano coating material.
Compared with the prior art, the invention has the beneficial effects that:
in the invention, nano SiO 2 The nano SiO is used as an inorganic filler 2 The comprehensive corrosion resistance of the coating can be obviously improved when the coating is used as the coating. However, the nano SiO 2 When the hexamethyldisilazane is applied to the nano SiO, the problems of insufficient hydrophobicity and dispersibility exist 2 After grafting modification is carried out, nano SiO can be further increased 2 Density of functionalized groups on the surface. According to the similar compatibility principle, the nano SiO can be improved 2 The dispersibility in the oily anti-corrosive pigment;
the cleaning and self-cleaning performance of the coating is realized by the application of nano SiO 2 The modification is carried out. By adding a low surface energy substance into the coating and improving the hydrophobic property of the substance, the self-cleaning effect of the substance is further improved. The n-octyl triethoxysilane not only has a lower surface energy, but also is SiO-based 2 The hydroxyl on the surface and the organic group with low surface energy of the n-octyl triethoxysilane are subjected to dehydration condensation reaction, so that the nano SiO subjected to secondary modification 2 The hydrophilic surface rich in hydroxyl is changed into the hydrophobic surface containing organic functional groups, thereby improving the nano SiO 2 Self-cleaning property of (1);
the secondary modified nano SiO 2 Mixing the epoxy resin, the fluorocarbon resin and the curing agent dicyandiamide to prepare the anticorrosive clean-keeping nano coating material. Wherein, the epoxy resin has high heat resistance and chemical resistance; the fluorocarbon resin takes C-F bond as a frameworkSo that the composite material has the advantage of high chemical stability. Epoxy resin, fluorocarbon resin and secondary modified nano SiO 2 The coating material with stable chemical property, high corrosion resistance and self-cleaning performance can be prepared by mixing.
Drawings
FIG. 1 is a process flow diagram of the present invention for preparing nano coating material for corrosion protection and sanitation;
FIG. 2 is a line graph of salt spray time data for a coating made according to the present invention;
FIG. 3 is a line graph of water contact angle data for coatings prepared in accordance with the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to 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, rather than all embodiments, and all other embodiments obtained by a person of ordinary skill in the art without any creative work based on the embodiments of the present invention belong to the protection scope of the present invention.
Example 1
A preparation method of an anticorrosive clean-keeping nano coating material comprises the following steps:
step one, stirring and mixing hexamethyldisilazane and an ethanol water solution to obtain a mixed solution; mixing nano SiO 2 Adding the mixture into the mixed solution, stirring and mixing the mixture, and drying the mixture in vacuum to obtain modified nano SiO 2 ；
Wherein, the nano SiO 2 The mixing mass ratio of the hexamethyldisilazane to the ethanol aqueous solution is 80;
stirring and mixing n-octyl triethoxysilane and an ethanol water solution according to the volume ratio of 1; adding ammonia water and modified nano SiO into the dissolved n-octyl triethoxysilane 2 Stirring, mixing and ultrasonic separatingDispersing to obtain dispersed SiO 2 A solution;
wherein, the modified nano SiO 2 The mass ratio of the hydrolyzed n-octyl triethoxysilane to the ammonia water is 3; the stirring and mixing conditions are as follows: the stirring and mixing speed is 300r/min, and the stirring and mixing time is 2h; the conditions of ultrasonic dispersion are as follows: the ultrasonic frequency is 500W, and the ultrasonic dispersion time is 30min; the ammonia water is 15wt% and is mixed with deionized water according to the volume ratio of 15;
step three, dispersing the SiO 2 Carrying out water bath reaction on the solution, and centrifuging to obtain a centrifuged product; drying and grinding the centrifuged product to obtain secondarily modified nano SiO 2 Powder;
wherein the temperature of the water bath reaction is 40 ℃, the time of the water bath reaction is 12h, the stirring speed of the water bath reaction is 300r/min, and the drying condition is drying for 5h at the temperature of 50 ℃;
step four, carrying out secondary modification on the nano SiO 2 The powder, the epoxy resin powder, the fluorocarbon resin powder and the dicyandiamide powder are uniformly mixed and dispersed according to the mass ratio of 10.
Example 2
A preparation method of an anticorrosive clean-keeping nano coating material comprises the following steps:
step one, stirring and mixing hexamethyldisilazane and an ethanol water solution to obtain a mixed solution; mixing nano SiO 2 Adding the mixture into the mixed solution, stirring and mixing the mixture, and drying the mixture in vacuum to obtain modified nano SiO 2 ；
Wherein, the nano SiO 2 The mixing mass ratio of the hexamethyldisilazane to the ethanol aqueous solution is 83;
stirring and mixing n-octyl triethoxysilane and an ethanol water solution according to the volume ratio of 1; adding ammonia water and modifier into dissolved n-octyl triethoxysilaneNano SiO of nature 2 Stirring, mixing and ultrasonic dispersing to obtain dispersed SiO 2 A solution;
wherein, the modified nano SiO 2 The mass ratio of the hydrolyzed n-octyl triethoxysilane to the ammonia water is 3; the conditions for stirring and mixing are as follows: the stirring and mixing speed is 500r/min, and the stirring and mixing time is 1h; the conditions of ultrasonic dispersion are as follows: the ultrasonic frequency is 500W, and the ultrasonic dispersion time is 60min; the ammonia water is 17wt% and is mixed with deionized water according to the volume ratio of 16;
step three, dispersing the SiO 2 Carrying out water bath reaction on the solution, and centrifuging to obtain a centrifuged product; drying and grinding the centrifuged product to obtain the secondary modified nano SiO 2 A powder;
wherein the temperature of the water bath reaction is 45 ℃, the time of the water bath reaction is 12h, the stirring speed of the water bath reaction is 400r/min, and the drying condition is drying for 3h at the temperature of 70 ℃;
step four, carrying out secondary modification on the nano SiO 2 The powder, the epoxy resin powder, the fluorocarbon resin powder and the dicyandiamide powder are uniformly mixed and dispersed according to the mass ratio of 15.
Example 3
A preparation method of an anticorrosive clean-keeping nano coating material comprises the following steps:
step one, stirring and mixing hexamethyldisilazane and an ethanol water solution to obtain a mixed solution; mixing nano SiO 2 Adding the mixture into the mixed solution, stirring and mixing the mixture, and drying the mixture in vacuum to obtain modified nano SiO 2 ；
Wherein, the nano SiO 2 The mixing mass ratio of hexamethyldisilazane to ethanol aqueous solution is 86;
stirring and mixing n-octyl triethoxysilane and an ethanol water solution according to the volume ratio of 1; to dissolveAdding ammonia water and modified nano SiO into the n-octyl triethoxysilane 2 Stirring, mixing and ultrasonic dispersing to obtain dispersed SiO 2 A solution;
wherein, the modified nano SiO 2 The mass ratio of the hydrolyzed n-octyltriethoxysilane to the ammonia water is 7; the conditions for stirring and mixing are as follows: the stirring and mixing speed is 400r/min, and the stirring and mixing time is 1.5h; the conditions of ultrasonic dispersion are as follows: the ultrasonic frequency is 500W, and the ultrasonic dispersion time is 45min; the ammonia water is 19wt% and is mixed with deionized water according to the volume ratio of 17;
step three, dispersing the SiO 2 Carrying out water bath reaction on the solution, and centrifuging to obtain a centrifuged product; drying and grinding the centrifuged product to obtain the secondary modified nano SiO 2 A powder;
wherein the temperature of the water bath reaction is 42 ℃, the time of the water bath reaction is 12 hours, the stirring speed of the water bath reaction is 350r/min, and the drying condition is drying for 4 hours at the temperature of 60 ℃;
step four, carrying out secondary modification on the nano SiO 2 The powder, the epoxy resin powder, the fluorocarbon resin powder and the dicyandiamide powder are uniformly mixed and dispersed according to the mass ratio of 17.
Example 4
A preparation method of an anticorrosive clean-keeping nano coating material comprises the following steps:
step one, stirring and mixing hexamethyldisilazane and an ethanol water solution to obtain a mixed solution; mixing nano SiO 2 Adding the mixture into the mixed solution, stirring and mixing the mixture, and drying the mixture in vacuum to obtain modified nano SiO 2 ；
Wherein, the nano SiO 2 The mixing mass ratio of the hexamethyldisilazane to the ethanol aqueous solution is 90;
step two, stirring and mixing the n-octyl triethoxysilane and the ethanol water solution according to the volume ratio of 1,obtaining hydrolyzed n-octyl triethoxysilane; adding ammonia water and modified nano SiO into the dissolved n-octyl triethoxysilane 2 Stirring, mixing and ultrasonic dispersing to obtain dispersed SiO 2 A solution;
wherein, the modified nano SiO 2 The mass ratio of the hydrolyzed n-octyl triethoxysilane to the ammonia water is 10; the stirring and mixing conditions are as follows: the stirring and mixing speed is 400r/min, and the stirring and mixing time is 1.5h; the ultrasonic dispersion conditions are as follows: the ultrasonic frequency is 500W, and the ultrasonic dispersion time is 45min; the ammonia water is 21wt% and is mixed with deionized water according to the volume ratio of 18;
step three, dispersing the SiO 2 Carrying out water bath reaction on the solution, and centrifuging to obtain a centrifuged product; drying and grinding the centrifuged product to obtain secondarily modified nano SiO 2 Powder;
wherein the temperature of the water bath reaction is 42 ℃, the time of the water bath reaction is 12h, the stirring speed of the water bath reaction is 350r/min, and the drying condition is drying for 4h at the temperature of 60 ℃;
step four, carrying out secondary modification on the nano SiO 2 The powder, the epoxy resin powder, the fluorocarbon resin powder and the dicyandiamide powder are uniformly mixed and dispersed according to the mass ratio of 20.
Example 5
A preparation method of an anticorrosive clean-keeping nano coating material comprises the following steps:
step one, stirring and mixing hexamethyldisilazane and an ethanol water solution to obtain a mixed solution; mixing nano SiO 2 Adding the mixture into the mixed solution, stirring and mixing the mixture, and drying the mixture in vacuum to obtain modified nano SiO 2 ；
Wherein, the nano SiO 2 The mixing mass ratio of hexamethyldisilazane to ethanol aqueous solution is 95;
step two, n-octyl triethoxy siliconStirring and mixing the alkyl and the ethanol water solution according to the volume ratio of 1; adding ammonia water and modified nano SiO into the dissolved n-octyl triethoxysilane 2 Stirring, mixing and ultrasonic dispersing to obtain dispersed SiO 2 A solution;
wherein, the modified nano SiO 2 The mass ratio of the hydrolyzed n-octyl triethoxysilane to the ammonia water is 12; the conditions for stirring and mixing are as follows: the stirring and mixing speed is 400r/min, and the stirring and mixing time is 1.5h; the conditions of ultrasonic dispersion are as follows: the ultrasonic frequency is 500W, and the ultrasonic dispersion time is 45min; the ammonia water is 23wt% and is mixed with deionized water according to the volume ratio of 19;
step three, dispersing the SiO 2 Carrying out water bath reaction on the solution, and centrifuging to obtain a centrifuged product; drying and grinding the centrifuged product to obtain the secondary modified nano SiO 2 Powder;
wherein the temperature of the water bath reaction is 42 ℃, the time of the water bath reaction is 12h, the stirring speed of the water bath reaction is 350r/min, and the drying condition is drying for 4h at the temperature of 60 ℃;
step four, carrying out secondary modification on the nano SiO 2 The powder, the epoxy resin powder, the fluorocarbon resin powder and the dicyandiamide powder are uniformly mixed and dispersed according to the mass ratio of 25.
Example 6
A preparation method of an anticorrosive clean-keeping nano coating material comprises the following steps:
step one, stirring and mixing hexamethyldisilazane and an ethanol water solution to obtain a mixed solution; mixing nano SiO 2 Adding the mixture into the mixed solution, stirring and mixing the mixture, and drying the mixture in vacuum to obtain modified nano SiO 2 ；
Wherein, the nano SiO 2 The mixing mass ratio of hexamethyldisilazane to ethanol aqueous solution is 100;
stirring and mixing n-octyltriethoxysilane and an ethanol water solution according to a volume ratio of 1; adding ammonia water and modified nano SiO into the dissolved n-octyl triethoxysilane 2 Stirring, mixing and ultrasonic dispersing to obtain dispersed SiO 2 A solution;
wherein, the modified nano SiO 2 The mass ratio of the hydrolyzed n-octyl triethoxysilane to the ammonia water is 15; the stirring and mixing conditions are as follows: the stirring and mixing speed is 400r/min, and the stirring and mixing time is 1.5h; the ultrasonic dispersion conditions are as follows: the ultrasonic frequency is 500W, and the ultrasonic dispersion time is 45min; the ammonia water is 25wt% and is mixed with deionized water according to the volume ratio of 20;
step three, dispersing the SiO 2 Carrying out water bath reaction on the solution, and centrifuging to obtain a centrifuged product; drying and grinding the centrifuged product to obtain secondarily modified nano SiO 2 A powder;
wherein the temperature of the water bath reaction is 42 ℃, the time of the water bath reaction is 12 hours, the stirring speed of the water bath reaction is 350r/min, and the drying condition is drying for 4 hours at the temperature of 60 ℃;
step four, carrying out secondary modification on the nano SiO 2 The powder, the epoxy resin powder, the fluorocarbon resin powder and the dicyandiamide powder are uniformly mixed and dispersed according to the mass ratio of 30.
Comparative example 1
A preparation method of an anticorrosive clean-keeping nano coating material comprises the following steps:
stirring and mixing n-octyl triethoxysilane and an ethanol water solution according to a volume ratio of 1; adding ammonia water and nano SiO into the dissolved n-octyl triethoxysilane 2 Stirring, mixing and ultrasonic dispersing to obtain dispersed SiO 2 A solution;
wherein, the nano SiO 2 The mass ratio of the hydrolyzed n-octyltriethoxysilane to the ammonia water is 3; stirring mixed barThe parts are as follows: the stirring and mixing speed is 300r/min, and the stirring and mixing time is 2h; the conditions of ultrasonic dispersion are as follows: the ultrasonic frequency is 500W, and the ultrasonic dispersion time is 30min; the ammonia water is 15wt% and is mixed with deionized water according to the volume ratio of 15;
step two, dispersing the SiO 2 Carrying out water bath reaction on the solution, and centrifuging to obtain a centrifuged product; drying and grinding the centrifuged product to obtain modified nano SiO 2 A powder;
wherein the temperature of the water bath reaction is 40 ℃, the time of the water bath reaction is 12 hours, the stirring speed of the water bath reaction is 300r/min, and the drying condition is drying for 5 hours at the temperature of 50 ℃;
step three, modifying the nano SiO 2 The powder, the epoxy resin powder, the fluorocarbon resin powder and the dicyandiamide powder are uniformly mixed and dispersed according to the mass ratio of 10.
Comparative example 2
A preparation method of an anticorrosive clean-keeping nano coating material comprises the following steps:
step one, stirring and mixing hexamethyldisilazane and an ethanol water solution to obtain a mixed solution; mixing nano SiO 2 Adding the mixture into the mixed solution, stirring and mixing the mixture, and drying the mixture in vacuum to obtain modified nano SiO 2 ；
Wherein, the nano SiO 2 The mixing mass ratio of the hexamethyldisilazane to the ethanol aqueous solution is 80;
stirring and mixing n-octyltriethoxysilane and an ethanol water solution according to a volume ratio of 1; adding ammonia water and modified nano SiO into dissolved n-octyl triethoxysilane 2 Stirring, mixing and ultrasonic dispersing to obtain dispersed SiO 2 A solution;
wherein, the modified nano SiO 2 Of hydrolyzed n-octyltriethoxysilane and aqueous ammoniaThe mass ratio is 3; the stirring and mixing conditions are as follows: the stirring and mixing speed is 300r/min, and the stirring and mixing time is 2h; the conditions of ultrasonic dispersion are as follows: the ultrasonic frequency is 500W, and the ultrasonic dispersion time is 30min; the ammonia water is 15wt% and is mixed with deionized water according to the volume ratio of 15;
step three, dispersing the SiO 2 Carrying out water bath reaction on the solution, and centrifuging to obtain a centrifuged product; drying and grinding the centrifuged product to obtain secondarily modified nano SiO 2 A powder;
wherein the temperature of the water bath reaction is 40 ℃, the time of the water bath reaction is 12 hours, the stirring speed of the water bath reaction is 300r/min, and the drying condition is drying for 5 hours at the temperature of 50 ℃;
step four, carrying out secondary modification on the nano SiO 2 And uniformly mixing and dispersing the powder, the epoxy resin powder and the dicyandiamide powder according to the mass ratio of 10.
Comparative example 3
A preparation method of an anticorrosive clean-keeping nano coating material comprises the following steps:
step one, stirring and mixing hexamethyldisilazane and an ethanol water solution to obtain a mixed solution; mixing nano SiO 2 Adding the mixture into the mixed solution, stirring and mixing the mixture, and drying the mixture in vacuum to obtain modified nano SiO 2 ；
Wherein, the nano SiO 2 The mixing mass ratio of the hexamethyldisilazane to the ethanol aqueous solution is 80;
step two, modifying the nano SiO 2 The powder, the epoxy resin powder, the fluorocarbon resin powder and the dicyandiamide powder are uniformly mixed and dispersed according to the mass ratio of 10.
Nano SiO adopted in the invention 2 From Jiangsu Tianxing New materials Co., ltd, the model is TSP-L12; the hexamethyldisilazane is from Wuhan Huaxiang biotechnology, inc. typeHXKJ, cat number HX8422A; n-octyl triethoxysilane is available from Jinan Yuancheng chemical Co., ltd, cat # 0953; the epoxy resin is bisphenol A type epoxy resin E51, is powder, is from a special chemical shop of Nantong star, and has a product number of 17; the fluorocarbon resin is from Guangdong Jiangsu Wenzui chemical reagent company Limited, and is in powder form, and the product number is PB93153; dicyandiamide is available from soaring chemical company Limited in Jinan, in powder form, with the code AOX68.
The coating materials prepared in the examples 1-6 and the comparative examples 1-3 are uniformly sprayed on the surface of the ceramic, the spraying thickness is 5m, and after curing, performance test is carried out;
testing one: the salt spray was allowed to settle to the ceramic surface of the spray coating by spraying a brine containing 5wt% sodium chloride at a pH of 7.0 through a spray device, and the salt spray resistance time was recorded for each sample, with the test results shown in table 1:
TABLE 1
As can be seen from the test results in Table 1, the salt spray resistance times of examples 5-6 were prolonged as compared to examples 1-3 and the comparative example. Wherein the salt spray resistance time of both examples 5 and 6 exceeded 2200h. Nano SiO 2 After the hexamethyldisilazane is modified, the nano SiO is obviously improved 2 The dispersion in the coating material further improves the corrosion resistance of the coating material. Since comparative example 1 is not to nano SiO 2 Modified by hexamethyldisilazane, the salt spray resistance time is reduced compared with the example; comparative example 2 no fluorocarbon resin was added, and the fluorocarbon resin had strong corrosion resistance, so comparative example 2 had a shorter salt spray resistance time than example 1.
And (2) testing: detecting the wetting property, namely testing the contact angle of the ceramic surface sprayed with the coating material by using a DSA100 type contact angle measuring instrument of Germany KRUSS company; when the measurement is carried out, the water drop size is 10uL, the final result is the average value of five test results, and the test results are shown in table 2;
TABLE 2
According to the test results in Table 2, the nano SiO modified by n-octyl triethoxysilane 2 Due to the fact that the existence of hydrophilic hydroxyl groups and the introduction of hydrophobic organic functional groups are reduced, the self-cleaning performance of the prepared samples in each embodiment is improved, namely the hydrophobic performance is enhanced, and the water contact angle degree of the prepared samples is increased. The water contact angle degrees of examples 1-6 all exceeded 150 °; among them, example 6 has the largest water contact angle number of 167.3 °. While the modified nano SiO in comparative example 3 2 Without the secondary modification with n-octyltriethoxysilane, the hydrophilicity was reduced compared to each example, and the degree of water contact angle became smaller.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (10)
1. A preparation method of an anticorrosive clean-keeping nano coating material is characterized by comprising the following steps:
step one, stirring and mixing hexamethyldisilazane and an ethanol water solution to obtain a mixed solution; mixing nano SiO 2 Adding the mixture into the mixed solution, stirring and mixing the mixture, and drying the mixture in vacuum to obtain modified nano SiO 2 ；
Stirring and mixing n-octyl triethoxysilane and an ethanol water solution to obtain hydrolyzed n-octyl triethoxysilane; adding ammonia water and modified nano SiO into the dissolved n-octyl triethoxysilane 2 Stirring, mixing and ultrasonic dispersing to obtain dispersed SiO 2 A solution;
step three, dispersing the SiO 2 Carrying out water bath reaction on the solution, and centrifuging to obtain a centrifuged product; drying and grinding the centrifuged productTo obtain the secondary modified nano SiO 2 Powder;
step four, carrying out secondary modification on the nano SiO 2 The powder, the epoxy resin powder, the fluorocarbon resin powder and the dicyandiamide powder are mixed and dispersed evenly to obtain the anticorrosion clean-keeping nano coating material.
2. The method of claim 1, wherein in the first step, the nano SiO 2 The mass ratio of the hexamethyldisilazane to the ethanol aqueous solution is (80-100) to (10-20) to 100-150.
3. The method according to claim 1, wherein in the first step, the stirring and mixing conditions are as follows: the stirring and mixing speed is 300-500r/min, and the stirring and mixing time is 1-2h.
4. The method according to claim 1, wherein in the first step, the temperature of vacuum drying is 50-60 ℃, the time of vacuum drying is 300-400min, and the vacuum degree is-0.05 to-0.08 MPa.
5. The method as claimed in claim 1, wherein in the second step, the n-octyltriethoxysilane and the ethanol aqueous solution are mixed in a volume ratio of 1.
6. The method according to claim 1, wherein in the second step, the stirring and mixing conditions are as follows: the stirring and mixing speed is 300-500r/min, and the stirring and mixing time is 1-2h; the conditions of ultrasonic dispersion are as follows: the ultrasonic frequency is 500W, and the ultrasonic dispersion time is 30-60min.
7. The method as claimed in claim 1, wherein in the second step, the modified nano SiO 2 The mass ratio of the hydrolyzed n-octyltriethoxysilane to the ammonia water is (3-15): 20;
the ammonia water is prepared by mixing high-concentration ammonia water and deionized water;
the volume ratio of the deionized water to the high-concentration ammonia water is (15-20) to 5;
the concentration of the high-concentration ammonia water is 15-25wt%.
8. The method according to claim 1, wherein in the third step, the temperature of the water bath reaction is 40-45 ℃, the time of the water bath reaction is 12h, the stirring speed of the water bath reaction is 300-400r/min, and the drying condition is that the drying is performed at the temperature of 50-70 ℃ for 3-5h.
9. The method of claim 1, wherein in the fourth step, the nano SiO modified twice 2 The mass ratio of the powder to the epoxy resin powder to the fluorocarbon resin powder to the dicyandiamide powder is (10-30): 80, (5-20): 10.
10. An anticorrosive clean-keeping nano-coating material prepared by the method for preparing the anticorrosive clean-keeping nano-coating material according to any one of claims 1 to 9.
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