CN111777917A - Preparation method of modified etched basalt scale/epoxy resin composite coating - Google Patents
Preparation method of modified etched basalt scale/epoxy resin composite coating Download PDFInfo
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- CN111777917A CN111777917A CN202010559194.4A CN202010559194A CN111777917A CN 111777917 A CN111777917 A CN 111777917A CN 202010559194 A CN202010559194 A CN 202010559194A CN 111777917 A CN111777917 A CN 111777917A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/28—Compounds of silicon
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/04—Physical treatment, e.g. grinding, treatment with ultrasonic vibrations
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/12—Treatment with organosilicon compounds
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/08—Anti-corrosive paints
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
- C09D7/62—Additives non-macromolecular inorganic modified by treatment with other compounds
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/70—Additives characterised by shape, e.g. fibres, flakes or microspheres
Abstract
The invention discloses a preparation method of a modified etched basalt scale/epoxy resin composite coating, aiming at the situation that the basalt scale contains about 50 wt.% SiO2Using concentrated alkali solution and SiO2And (3) reacting, chemically etching the surface of the basalt scale, and modifying the basalt scale by using a silane coupling agent to form a chemical bonding interface on the modified and etched basalt/resin interface. By controlling the concentration, the etching reaction temperature and the reaction time of NaOH solutionEtched surfaces of different microscopic geometries; and introducing Si-OH and KH550 of Si-O-C2H5Condensation reaction is carried out to form chemical bonds; dispersing the modified and etched basalt scales in epoxy resin, and performing ring-opening homopolymerization reaction on the amino group of KH550 chemically bonded on the surfaces of the scales and the epoxy resin to form chemical bonding; finally, chemical bonding is formed on the modified and etched basalt scale/epoxy resin interface, and the compatibility and the dispersibility of the scale filler in the resin are improved.
Description
Technical Field
The invention relates to the field of coating fillers made of modified etched basalt scales, in particular to a preparation method of a modified etched basalt scale/epoxy resin composite coating.
Background
In high-salt and high-humidity coastal areas and aggressive atmosphere industrial areas, the service cycle of the organic coating can be greatly shortened, and the swelling and hydrolysis of the coating can be accelerated in severe environments, so that the shielding performance of the coating is reduced. In order to improve the shielding performance of the coating, research and development of heavy anti-corrosion paint and research on the protection mechanism thereof are always the key problems of anti-corrosion coating research. The heavy-duty anticorrosive paint containing the flaky filler attracts people's attention as a high-efficiency heavy-duty anticorrosive paint.
In the heavy anti-corrosive coating containing the scaly filler, how to improve the bonding strength of the filler/resin interface is a main research problem of the scaly filler anti-corrosive coating. For the problem of interface bonding strength, there are several representative theories at present: mechanical interlocking theory proposed by MeBain and Hopkin, electrostatic theory proposed by deryagulin et al, wetting and acid-base theory of a.d. mclaren. The above theories are focused on the research of improving the secondary bond force of the coating/solid material interface, and with the deepening of research work, especially the development of various microscopic surface testing technologies, people gradually realize that the bond energy of the chemical bond existing in the coating/solid material interface action is far greater than that of the secondary bond, so that the coating/filler interface forms chemical bonding, and the improvement of the overall performance of the coating is greatly influenced.
The main component of the inorganic scale filler commonly used in the anticorrosive coating is oxide SiO2E.g., glass flakes, micaceous iron oxide, and basalt flakes, etc., wherein the basalt flakes contain about 50 wt.% SiO2The material has excellent mechanical performance, acid and alkali resistance, high and low temperature resistance, chemical stability and ultraviolet irradiation resistance. The untreated basalt scale has a smooth surface, only contains a small amount of hydroxyl, is not beneficial to chemical modification, causes poor compatibility with epoxy resin, is easy to generate coagulation phenomenon in a coating, and severely limits the shielding performance of the basalt heavy-duty anticorrosive coating because a resin/scale interface is a physical adsorption interface.
Disclosure of Invention
The invention aims to provide a preparation method of a modified etched basalt scale/epoxy resin composite coating, which can enhance the bonding strength of a filler/resin interface, fully exert the shielding effect of the coating to improve the anticorrosion effect, is easy to operate and is suitable for batch production.
The technical scheme of the invention is as follows:
a preparation method of a modified etched basalt scale/epoxy resin composite coating comprises the following specific steps:
(1) preparing chemically etched basalt scales;
a. measuring a certain amount of concentrated alkali liquor, and pouring into a polytetrafluoroethylene conical flask;
b. weighing a certain amount of basalt flakes, and pouring the basalt flakes into a conical flask;
c. placing the conical flask in an oil bath kettle at 120 ℃, heating and stirring for a period of time, and then cooling to room temperature; d. filtering the mixture, and washing the mixture for multiple times by using deionized water to ensure that the pH value of the basalt mixed solution is more than or equal to 5;
(2) preparing modified etched basalt scales;
a. measuring a certain amount of etched basalt flakes and a certain amount of deionized water, mixing, and pouring into a 500mL flask for stirring;
b. stirring for a period of time, and adding a certain amount of silane coupling agent;
c. placing the flask in a water bath kettle, heating and stirring for a period of time;
d. filtering the mixture, washing the mixture for multiple times by using deionized water to ensure that the pH value of the mixed solution is more than or equal to 5, and drying the obtained modified etched basalt;
(3) preparing a modified etched basalt flake/epoxy resin composite coating;
a. weighing 10g of organic solvent, and dissolving 35g of epoxy resin (E44);
b. measuring a certain amount of modified etched basalt scales, and adding the modified etched basalt scales and E44 into a 500mL agate mortar;
c. adding agate balls, and performing ball milling for 90min to obtain a well-dispersed modified etched basalt flake/epoxy resin liquid mixture;
d. 15g of a polyamide curing agent (651) was added to the mixture and applied to the pretreated carbon steel sheet to obtain a 120 μm coating after curing.
The preferable scheme of the preparation method of the modified etched basalt flake/epoxy resin composite coating is that in the step (1), the concentrated alkali solution is 2-4M mol/L NaOH solution.
The preferable scheme of the preparation method of the modified etched basalt scale/epoxy resin composite coating is that in the step (1), the basalt scale is 200-500-mesh basalt scale.
The preferable scheme of the preparation method of the modified etched basalt scale/epoxy resin composite coating is that in the step (1), the heating time of the oil bath is 1-3 hours.
The preparation method of the modified etched basalt scale/epoxy resin composite coating has the preferred scheme that in the step (2), the weight ratio of the etched basalt scale to deionized water is 1: 50-1: 30.
The preferable scheme of the preparation method of the modified etched basalt scale/epoxy resin composite coating is that in the step (2), the silane coupling agent is KH 550.
The preferable scheme of the preparation method of the modified etched basalt scale/epoxy resin composite coating is that in the step (2), the weight ratio of the etched basalt scale to KH550 is 5: 1-10: 1.
The preparation method of the modified etched basalt scale/epoxy resin composite coating has the preferred scheme that in the step (2), the heating temperature is 60-80 ℃, and the heating time is 1-3 hours.
The preferable scheme of the preparation method of the modified etched basalt scale/epoxy resin composite coating is that in the step (3), the weight ratio of the modified etched basalt scale to the E44 is 1: 5-1: 20.
In the present invention, since the basalt flakes contain about 50 wt.% SiO2Concentrated NaOH solution was used to react with SiO2, the equation is as follows:
obtaining etched surfaces with different micro-geometric structures by controlling the concentration of NaOH solution, the etching reaction temperature and the reaction time; and introducing Si-OH and KH550 of Si-O-C2H5Condensation reaction is carried out to form chemical bonds; dispersing the modified and etched basalt scales in epoxy resin, and performing ring-opening homopolymerization reaction on the amino group of KH550 chemically bonded on the surfaces of the scales and the epoxy resin to form chemical bonding; finally, chemical bonding is formed on the modified and etched basalt scale/epoxy resin interface, and the compatibility and the dispersibility of the scale filler in the resin are improved. The invention provides a good foundation for the subsequent research of inorganic scale pigment and filler, and has important significance for promoting the engineering application of the organic anticorrosive coating.
The invention has the beneficial effects that: the method is characterized in that the basalt scales are subjected to chemical etching activation treatment in advance, the roughness and the hydroxyl content of the surfaces of the scales are improved, organosilane is used as a bridging agent to carry out chemical grafting on the surfaces of the scales, the modified and etched basalt scales are added into epoxy resin, the series of chemical modification is verified through a settlement test and the microscopic appearance of the cross section of a coating, and the compatibility of the basalt scales and the epoxy resin is obviously improved.
Drawings
FIG. 1 is a schematic illustration of chemically etched, chemically modified basalt flakes;
FIG. 2 is an infrared spectrum of functional groups on the surface of a basalt scale before and after chemical etching of the scale;
FIG. 3 shows SEM images of the micro-morphology of basalt scales before and after chemical etching.
Fig. 4 electrochemical impedance spectra of epoxy coating, basalt flake/epoxy coating, and modified etched basalt flake/epoxy coating soaked in 3.5 wt.% NaCI solution for 240 hours.
Detailed Description
The present invention is further described in the following examples, which are intended to be illustrative of the best mode of carrying out the invention and are not intended to limit the scope of the invention in any way.
Preparing chemically etched basalt scales; a, measuring 800ml of 4mol/L concentrated NaOH solution, and pouring the solution into a 1000ml polytetrafluoroethylene conical flask; b, weighing 30g of basalt flakes, and pouring the basalt flakes into a conical flask; c, placing the conical flask in a 120 ℃ oil bath pot, heating and stirring for 2.5 hours, and then cooling to room temperature; and d, filtering the mixture, and washing the mixture for multiple times by using deionized water to ensure that the pH value of the basalt mixed solution is more than or equal to 5.
Preparing modified etched basalt scales; a, measuring 10 etched basalt scales and 350mL of deionized water, mixing, and pouring into a 500mL flask for stirring; b, stirring for 0.5h, and then adding 2.5g of silane coupling agent KH 550; c, placing the flask in a 75 ℃ water bath kettle, heating and stirring for 3 hours; and d, filtering the mixture, washing the mixture for multiple times by using deionized water to ensure that the pH value of the mixed solution is more than or equal to 5, and drying the obtained modified etched basalt.
Preparing a modified etched basalt flake/epoxy resin composite coating; a, measuring 10g of organic solvent, and dissolving 35g of epoxy resin (E44); b, measuring 10g of modified etched basalt scales, and adding the modified etched basalt scales and E44 into a 500mL agate mortar; c, adding agate balls, and performing ball milling treatment for 90min to obtain a well-dispersed modified etched basalt flake/epoxy resin liquid mixture; d adding 15g of polyamide curing agent (651) into the mixture, coating the mixture on the pretreated carbon steel sheet, and curing to obtain a coating with the thickness of 120 mu m.
As can be observed in FIG. 1, the basalt flakes must undergo an etching reaction in a polytetrafluoroethylene container, because the glass container reacts with concentrated alkali solution, and there is a high possibility that danger may occur during the etching reaction; etching reaction Si-OH with Si-O-of KH550C2H5Condensation reaction is carried out to form chemical bonds; and dispersing the modified and etched basalt scales in epoxy resin, and performing ring-opening homopolymerization reaction on the amino group of KH550 chemically bonded on the surfaces of the scales and the epoxy resin to form chemical bonding.
As shown in FIG. 2, the FT-IR curve of basalt flakes was 3500cm-1The peak at (A) is the stretching vibration of the hydroxyl group, 1000cm-1The peak is the bending peak of Si-O-Si, and the strength of the carboxyl peak is very small, which indicates that the chemical activity of the surface of the basalt flake is very low, and the surface contains few sites for chemical modification, thus being not beneficial to the chemical modification; the chemically etched basalt flakes have the same chemical functional groups in the FT-IR curve, but can be clearly seen at 1500cm-1Has a very obvious bending peak of hydroxyl, 3500cm-1The stretching vibration peak of the hydroxyl is obviously enhanced, which explains the chemical etching process, so that the surface of the basalt scale is activated, a plurality of hydroxyl is added, and the chemically etched basalt scale is easy to modify.
FIG. 3 is a SEM photograph: (a1, a2) magnified pictures of low and high magnification of basalt scales; (b1, b2) chemically etched basalt scale low and high magnification picture, it can be seen that the size of the unetched basalt scale is: the length and width are about 20-30 mu m, the thickness is about 2-3 mu m, and high-power photos show that the surfaces of the basalt scales are very smooth, which indicates that the adhesion of the basalt scales with resin in an organic coating is very low, and the compatibility is poor; after chemical etching, the size of the scale: the length and width are less than 20 mu m, the thickness is less than 2 mu m, and uniformly distributed micropores are formed on the surface, which can ensure that the scales form sawtooth occlusion effect with the resin in the coating and increase the bonding force of the resin/filler interface.
As can be seen from the Nyquist plot of the electrochemical impedance of the epoxy coating, the basalt/epoxy coating and the modified etched basalt/epoxy coating in FIG. 4, after soaking in corrosive media for 240 hours, the low-frequency impedance modulus of the epoxy coating is 6.59 × 1010Ω·cm2Down to 1.11 × 109Ω·cm2The low-frequency impedance modulus value of the basalt scale/epoxy coating is from 8.23 × 1010Ω·cm2Down to 1.88 × 1010Ω·cm2The low-frequency impedance modulus value of the modified etched basalt scale/epoxy coating is from 3.23 × 1011Ω·cm2Down to 1.19 × 1011Ω·cm2. Therefore, the corrosion resistance of the epoxy coating can be greatly improved after the basalt scales are subjected to chemical etching and chemical modification.
Claims (9)
1. A preparation method of a modified etched basalt scale/epoxy resin composite coating is characterized by comprising the following specific steps:
(1) preparing chemically etched basalt scales;
a. measuring a certain amount of concentrated alkali liquor, and pouring into a polytetrafluoroethylene conical flask;
b. weighing a certain amount of basalt flakes, and pouring the basalt flakes into a conical flask;
c. placing the conical flask in an oil bath kettle at 120 ℃, heating and stirring for a period of time, and then cooling to room temperature;
d. filtering the mixture, and washing the mixture for multiple times by using deionized water to ensure that the pH value of the basalt mixed solution is more than or equal to 5;
(2) preparing modified etched basalt scales;
a. measuring a certain amount of etched basalt flakes and a certain amount of deionized water, mixing, and pouring into a 500mL flask for stirring;
b. stirring for a period of time, and adding a certain amount of silane coupling agent;
c. placing the flask in a water bath kettle, heating and stirring for a period of time;
d. filtering the mixture, washing the mixture for multiple times by using deionized water to ensure that the pH value of the mixed solution is more than or equal to 5, and drying the obtained modified etched basalt;
(3) preparing a modified etched basalt flake/epoxy resin composite coating;
a. weighing 10g of organic solvent, and dissolving 35g of epoxy resin (E44);
b. measuring a certain amount of modified etched basalt scales, and adding the modified etched basalt scales and E44 into a 500mL agate mortar;
c. adding agate balls, and performing ball milling for 90min to obtain a well-dispersed modified etched basalt flake/epoxy resin liquid mixture;
d. 15g of a polyamide curing agent (651) was added to the mixture and applied to the pretreated carbon steel sheet to obtain a 120 μm coating after curing.
2. The preparation method of the modified etched basalt scale/epoxy resin composite coating, as claimed in claim 1, wherein: in the step (1), the concentrated alkali solution is 2-4 mol/L NaOH solution.
3. The preparation method of the modified etched basalt scale/epoxy resin composite coating, as claimed in claim 1, wherein: in the step (1), the basalt scales are 200-500-mesh basalt scales.
4. The preparation method of the modified etched basalt scale/epoxy resin composite coating, as claimed in claim 1, wherein: in the step (1), the heating time of the oil bath is 1-3 hours.
5. The preparation method of the modified etched basalt scale/epoxy resin composite coating, as claimed in claim 1, wherein: in the step (2), the weight ratio of the etched basalt scales to the deionized water is 1: 50-1: 30.
6. The preparation method of the modified etched basalt scale/epoxy resin composite coating, as claimed in claim 1, wherein: in the step (2), the silane coupling agent is KH 550.
7. The preparation method of the modified etched basalt scale/epoxy resin composite coating, as claimed in claim 1, wherein: in the step (2), the weight ratio of the etched basalt scales to the KH550 is 5: 1-10: 1.
8. The preparation method of the modified etched basalt scale/epoxy resin composite coating, as claimed in claim 1, wherein: in the step (2), the heating temperature is 60-80 ℃, and the heating time is 1-3 hours.
9. The preparation method of the modified etched basalt scale/epoxy resin composite coating, as claimed in claim 1, wherein: in the step (3), the weight ratio of the modified etched basalt scales to the E44 is 1: 5-1: 20.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114591677A (en) * | 2022-03-31 | 2022-06-07 | 陕西科技大学 | Basalt nanosheet-based super-hydrophobic coating material and preparation method thereof |
| CN115819845A (en) * | 2022-12-23 | 2023-03-21 | 国网浙江省电力有限公司金华供电公司 | Filler modification method, modified filler and filled heat-conducting epoxy resin |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107384118A (en) * | 2017-06-15 | 2017-11-24 | 东南大学 | Modified basalt scale solvent-free epoxy resin anticorrosive paint and preparation method thereof |
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2020
- 2020-06-18 CN CN202010559194.4A patent/CN111777917A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107384118A (en) * | 2017-06-15 | 2017-11-24 | 东南大学 | Modified basalt scale solvent-free epoxy resin anticorrosive paint and preparation method thereof |
Non-Patent Citations (1)
| Title |
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| 李静等: "酸刻蚀对玄武岩纤维表面偶联剂吸附量及纤维／环氧树脂复合材料力学性能的影响", 《复合材料学报》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114591677A (en) * | 2022-03-31 | 2022-06-07 | 陕西科技大学 | Basalt nanosheet-based super-hydrophobic coating material and preparation method thereof |
| CN114591677B (en) * | 2022-03-31 | 2023-03-10 | 陕西科技大学 | Basalt nanosheet-based super-hydrophobic coating material and preparation method thereof |
| CN115819845A (en) * | 2022-12-23 | 2023-03-21 | 国网浙江省电力有限公司金华供电公司 | Filler modification method, modified filler and filled heat-conducting epoxy resin |
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