CN113637380A - Preparation method of graphene oxide-silicon nitride composite powder/urushiol formal composite coating - Google Patents
Preparation method of graphene oxide-silicon nitride composite powder/urushiol formal composite coating Download PDFInfo
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- CN113637380A CN113637380A CN202110993911.9A CN202110993911A CN113637380A CN 113637380 A CN113637380 A CN 113637380A CN 202110993911 A CN202110993911 A CN 202110993911A CN 113637380 A CN113637380 A CN 113637380A
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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
- C09D161/00—Coating compositions based on condensation polymers of aldehydes or ketones; Coating compositions based on derivatives of such polymers
- C09D161/04—Condensation polymers of aldehydes or ketones with phenols only
- C09D161/06—Condensation polymers of aldehydes or ketones with phenols only of aldehydes with phenols
- C09D161/12—Condensation polymers of aldehydes or ketones with phenols only of aldehydes with phenols with polyhydric phenols
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G8/00—Condensation polymers of aldehydes or ketones with phenols only
- C08G8/04—Condensation polymers of aldehydes or ketones with phenols only of aldehydes
- C08G8/08—Condensation polymers of aldehydes or ketones with phenols only of aldehydes of formaldehyde, e.g. of formaldehyde formed in situ
- C08G8/20—Condensation polymers of aldehydes or ketones with phenols only of aldehydes of formaldehyde, e.g. of formaldehyde formed in situ with polyhydric phenols
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- 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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Abstract
The invention relates to a preparation method of graphene oxide-silicon nitride composite powder/urushiol formal composite coating, wherein Si-OH bonds generated by hydrolysis of Si-O bonds on a silane coupling agent react with active groups such as a large amount of hydroxyl groups on the surfaces of graphene oxide and silicon nitride to modify and graft the silane coupling agent, the graphene oxide and the silicon nitride together, so that KSi is obtained3N4KGO composite powder, which contains a large amount of organic chain segment and is compatible with the oily chain segment structure in urushiol formal resin, so as to prepare a composite powder with high hardness, strong adhesion, no toxicity, no sensitization and corrosion resistance after film formingThe composite coating has the characteristic of excellent performance.
Description
Technical Field
The invention relates to the technical field of coatings, in particular to a preparation method of a graphene oxide-silicon nitride composite powder/urushiol formal composite coating.
Background
The raw lacquer is the secretion of natural lacquer tree, has excellent durability and decoration, and is a name of 'the king of coating' in China.
However, the raw lacquer has major application obstacles such as high viscosity, unsuitable construction, and harsh drying requirements, so that the raw lacquer cannot meet the production and construction requirements since the modern time, and the demand of modification treatment on the raw lacquer is more and more urgent.
Disclosure of Invention
Aiming at the problems, the preparation method of the graphene oxide-silicon nitride composite powder/urushiol formal composite coating is provided, and the problem of poor film forming property of the urushiol formal is effectively solved.
The specific technical scheme is as follows:
the first aspect of the invention provides a preparation method of a graphene oxide-silicon nitride composite powder/urushiol formal composite coating, which is characterized by comprising the following steps:
1) uniformly mixing a urushiol xylene solution, a formaldehyde solution, ammonia water and tetrabutylammonium chloride in a mass ratio of 100:10:1:2, then heating to 90-100 ℃, carrying out heat preservation reaction for 2 hours, then continuously heating to 145-9000 mPa.s, carrying out heat preservation stirring reaction until a certain viscosity is reached, and stopping the reaction to obtain a urushiol formal solution;
2) uniformly mixing absolute ethyl alcohol, distilled water and a silane coupling agent KH-560 according to the mass ratio of 18:0.5:2, adding 1 wt% of graphene oxide into the feed liquid, performing ultrasonic dispersion uniformly, keeping the temperature at 80 ℃, stirring for 5-7h, centrifuging, washing, vacuum drying and grinding to obtain modified graphene oxide;
3) uniformly mixing absolute ethyl alcohol, distilled water and a silane coupling agent KH-550 in a mass ratio of 18:0.5:2, adding 1 wt% of silicon nitride into the feed liquid, performing ultrasonic dispersion uniformly, keeping the temperature at 80 ℃, stirring for 5-7 hours, centrifuging, washing, vacuum drying and grinding to obtain modified silicon nitride;
4) ultrasonically dispersing the modified graphene oxide prepared in the step 2) and the modified silicon nitride prepared in the step 3) in N, N-dimethylformamide, then carrying out heat preservation and stirring reaction at 120 ℃ for 6 hours, centrifuging, washing, vacuum drying and grinding to obtain modified graphene oxide-silicon nitride composite powder;
5) adding the graphene oxide-silicon nitride composite powder prepared in the step 4) into the urushiol formal solution prepared in the step 1), and uniformly stirring and mixing to obtain the modified graphene oxide-silicon nitride composite powder/urushiol formal composite coating.
The above-mentioned production method is also characterized in that the mass fraction of the urushiol xylene solution in the step 1) is 38 to 40%.
The above preparation method is also characterized in that the addition amounts of the modified graphene oxide and the modified silicon nitride in step 4) are both 10 wt% based on the mass of the N, N-dimethylformamide.
The preparation method is also characterized in that the addition amount of the graphene oxide-silicon nitride composite powder in the step 5) is 0.5-1 wt% based on the mass of the urushiol formal solution.
The second aspect of the invention provides a graphene oxide-silicon nitride composite powder/urushiol formal composite coating prepared by the preparation method.
In the invention, Si-OH bonds generated by hydrolysis of Si-O bonds on silane coupling agent, Graphene Oxide (GO) and silicon nitride (Si)3N4) The surface of the polymer contains a large number of active groups such as hydroxyl groups and the like to react so as to modify and graft the silane coupling agent, the graphene oxide and the silicon nitride together, thereby obtaining the KSi3N4KGO composite powder, which contains a large amount of organic segments and is compatible with the oily segment structure of urushiol formal resin.
The beneficial effect of above-mentioned scheme is:
1) in the invention, phase catalyst tetrabutyl ammonium chloride is introduced, so that the synthetic reaction of urushiol formal is more sufficient;
2) the paint film prepared by the invention has the characteristics of high hardness, strong adhesive force, no toxicity after film forming, no sensitization and excellent corrosion resistance.
Drawings
Fig. 1 is a contact angle diagram of a composite coating film provided in example 1 of 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 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 the embodiments and features of the embodiments may be combined with each other without conflict.
The invention is further described with reference to the following drawings and specific examples, which are not intended to be limiting.
Example 1
A graphene oxide-silicon nitride composite powder/urushiol formal composite coating is prepared by the following steps:
1) adding a urushiol xylene solution with the mass fraction of 38 wt%, a formaldehyde solution, ammonia water and tetrabutylammonium chloride into a three-neck flask according to the mass ratio of 100:10:1:2, uniformly mixing, heating to 95 ℃, keeping the temperature for reaction for 2 hours, continuing heating to 150 ℃, keeping the temperature, stirring for reaction until a certain viscosity is reached, and stopping the reaction to obtain a urushiol formal solution;
2) uniformly mixing absolute ethyl alcohol, distilled water and a silane coupling agent KH-560 according to the mass ratio of 18:0.5:2, adding 1 wt% of graphene oxide into the feed liquid, performing ultrasonic dispersion uniformly, performing heat preservation and stirring at 80 ℃ for 6 hours, centrifuging, washing, performing vacuum drying, and grinding to obtain nano-modified graphene oxide (KGO);
3) uniformly mixing absolute ethyl alcohol, distilled water and silane coupling agent KH-550 in a mass ratio of 18:0.5:2, and thenAdding 1 wt% of silicon nitride into the feed liquid, uniformly dispersing by ultrasonic, stirring for 5h at the temperature of 80 ℃, centrifuging, washing, drying in vacuum, and grinding to obtain the nano-grade modified silicon nitride (KSi)3N4)；
4) Ultrasonically dispersing the modified graphene oxide prepared in the step 2) and the modified silicon nitride prepared in the step 3) in N, N-dimethylformamide, then carrying out heat preservation and stirring reaction for 6 hours at 120 ℃, centrifuging, washing, vacuum drying and grinding to obtain modified graphene oxide-silicon nitride composite powder (KSi)3N4-KGO composite powder);
5) adding the graphene oxide-silicon nitride composite powder prepared in the step 4) into the urushiol formal solution prepared in the step 1) by 0.5 wt% of the addition amount, and stirring and mixing uniformly to obtain the modified graphene oxide-silicon nitride composite powder/urushiol formal composite coating.
In the present invention, no tetrabutylammonium chloride was added and the comparative example was prepared according to the preparation method described in step 1) of example 1.
The physical properties of the modified graphene oxide-silicon nitride composite powder/urushiol formal composite coating film and the urushiol formal solution coating film in the step 1) are shown in the following table:
as can be seen from the comparison of the above tables, 0.5% by weight of KSi was added in the present application compared with the urushiol formal coating film without additives3N4The coating hardness of the-KGO composite powder is improved to 4H, and the adhesive force is also improved to 1 grade, which shows that KSi3N4The introduction of the KGO composite powder can improve the hardness and the adhesive force of the coating to a certain extent, which is mainly characterized in that the attraction of the coating to the substrate is enhanced by a large amount of active groups on the surface of the nano composite powder; the hardness, flexibility and adhesive force of the urushiol formal coating film without the phase catalyst are lower than those of the urushiol formal coating film with the phase catalyst, mainly because the phase catalyst accelerates the polycondensation reaction, so that the obtained urushiol formal coating film has longer moleculesAnd the chain segment has higher crosslinking density and better mechanical property.
The overall mechanical property of the composite coating provided by the invention is improved to a certain extent, and the requirement of daily corrosion resistance can be met.
As can be seen from the comparison of FIG. 1, the urushiol formal coating film of the present invention is added with 0.5 wt% of GO, KGO, Si3N4，KSi3N4The contact angle of the coating film of the composite coating reaches the highest 95 degrees, which is mainly attributed to that KSi is successfully superposed with-Si-O-Si-hydrophobic chain segments introduced into composite powder3N4And KGO, thereby remarkably improving the hydrophobic property of the coating film.
Example 2
A graphene oxide-silicon nitride composite powder/urushiol formal composite coating is prepared by the following steps:
1) adding a urushiol xylene solution with the mass fraction of 38 wt%, a formaldehyde solution, ammonia water and tetrabutylammonium chloride into a three-neck flask according to the mass ratio of 100:10:1:2, uniformly mixing, heating to 95 ℃, keeping the temperature for reaction for 2 hours, continuing heating to 150 ℃, keeping the temperature, stirring for reaction until a certain viscosity is reached, and stopping the reaction to obtain a urushiol formal solution;
2) uniformly mixing absolute ethyl alcohol, distilled water and a silane coupling agent KH-560 according to the mass ratio of 18:0.5:2, adding 1 wt% of graphene oxide into the feed liquid, performing ultrasonic dispersion uniformly, performing heat preservation and stirring at 80 ℃ for 6 hours, centrifuging, washing, performing vacuum drying, and grinding to obtain nanoscale modified graphene oxide;
3) uniformly mixing absolute ethyl alcohol, distilled water and a silane coupling agent KH-550 in a mass ratio of 18:0.5:2, adding 1 wt% of silicon nitride into the feed liquid, performing ultrasonic dispersion uniformly, keeping the temperature at 80 ℃, stirring for 5 hours, centrifuging, washing, drying in vacuum, and grinding to obtain nano-modified silicon nitride;
4) ultrasonically dispersing the modified graphene oxide prepared in the step 2) and the modified silicon nitride prepared in the step 3) in N, N-dimethylformamide, then carrying out heat preservation and stirring reaction at 120 ℃ for 6 hours, centrifuging, washing, vacuum drying and grinding to obtain modified graphene oxide-silicon nitride composite powder;
5) adding the graphene oxide-silicon nitride composite powder prepared in the step 4) into the urushiol formal solution prepared in the step 1) by adding 1 wt% of the graphene oxide-silicon nitride composite powder, and uniformly stirring and mixing to obtain the modified graphene oxide-silicon nitride composite powder/urushiol formal composite coating.
The physical properties of the modified graphene oxide-silicon nitride composite powder/urushiol formal composite coating film and the urushiol formal solution coating film in the step 1) are shown in the following table:
in the invention, a small amount of water is found to exist in the system after the modification reaction when a powder modification test is carried out, and analysis shows that the small amount of water is mainly because the volatilization speed of absolute ethyl alcohol is very high, and the small amount of water can provide a large amount of hydrogen bonds on the surface of the powder, so that the modified system is lumpy due to the existence of the hydrogen bonds after drying treatment, and the modified powder is difficult to grind into a nano grade during subsequent grinding, thereby seriously influencing the subsequent tests in the steps 4) and 5). In view of the above, in the invention, attempts are made to increase the proportion of absolute ethyl alcohol and reduce the water consumption, so that the residual water in the system is reduced by utilizing the combined action of ethanol volatilization and the silane coupling agent.
While the invention has been described with reference to a preferred embodiment, it will be understood by those skilled in the art that various changes in form and detail may be made therein without departing from the spirit and scope of the invention.
Claims (5)
1. A preparation method of graphene oxide-silicon nitride composite powder/urushiol formal composite coating is characterized by comprising the following steps:
1) uniformly mixing the urushiol xylene solution, the formaldehyde solution, ammonia water and tetrabutylammonium chloride in a mass ratio of 100:10:1:2, then heating to 90-100 ℃, carrying out heat preservation reaction for 2 hours, then continuously heating to 145-160 ℃, carrying out heat preservation stirring reaction until certain viscosity is reached, and stopping reaction to obtain a urushiol formal solution;
2) uniformly mixing absolute ethyl alcohol, distilled water and a silane coupling agent KH-560 according to the mass ratio of 18:0.5:2, adding 1 wt% of graphene oxide into the feed liquid, performing ultrasonic dispersion uniformly, keeping the temperature at 80 ℃, stirring for 5-7h, centrifuging, washing, vacuum drying and grinding to obtain modified graphene oxide;
3) uniformly mixing absolute ethyl alcohol, distilled water and a silane coupling agent KH-550 in a mass ratio of 18:0.5:2, adding 1 wt% of silicon nitride into the feed liquid, performing ultrasonic dispersion uniformly, keeping the temperature at 80 ℃, stirring for 5-7 hours, centrifuging, washing, vacuum drying and grinding to obtain modified silicon nitride;
4) ultrasonically dispersing the modified graphene oxide prepared in the step 2) and the modified silicon nitride prepared in the step 3) in N, N-dimethylformamide, then carrying out heat preservation and stirring reaction at 120 ℃ for 6 hours, centrifuging, washing, vacuum drying and grinding to obtain modified graphene oxide-silicon nitride composite powder;
5) adding the graphene oxide-silicon nitride composite powder prepared in the step 4) into the urushiol formal solution prepared in the step 1), and uniformly stirring and mixing to obtain the modified graphene oxide-silicon nitride composite powder/urushiol formal composite coating.
2. The method according to claim 1, wherein the mass fraction of the urushiol xylene solution in step 1) is 38 to 40%.
3. The preparation method according to claim 1, wherein the modified graphene oxide and the modified silicon nitride are added in an amount of 10 wt% based on the mass of N, N-dimethylformamide in the step 4).
4. The preparation method according to claim 1, wherein the graphene oxide-silicon nitride composite powder is added in the amount of 0.5 to 1 wt% based on the mass of the urushiol formal solution in the step 5).
5. The graphene oxide-silicon nitride composite powder/urushiol formal composite coating is characterized by being prepared according to the preparation method of any one of claims 1 to 4.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1531181A (en) * | 1977-01-25 | 1978-11-01 | Nizhnetagilsky Z Plastmass | Method of producing novolac phenol-formaldehyde resins |
| US20180118645A1 (en) * | 2013-06-13 | 2018-05-03 | Empire Technology Development Llc | Multi-functional phenolic resins |
| CN107987661A (en) * | 2017-12-29 | 2018-05-04 | 西北农林科技大学 | A kind of biomass graphene modified raw lacquer heavy antisepsis composite coating and preparation method thereof |
| CN108659675A (en) * | 2018-05-23 | 2018-10-16 | 中国海洋大学 | A kind of preparation method of the Long-effect corrosion-resistant wave transparent coating of graphene modification silicon nitride |
| CN110499086A (en) * | 2019-07-19 | 2019-11-26 | 武汉理工大学 | A kind of silicon nitride comprising graphene oxide composite granule solventless epoxy coating and the preparation method and application thereof |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1531181A (en) * | 1977-01-25 | 1978-11-01 | Nizhnetagilsky Z Plastmass | Method of producing novolac phenol-formaldehyde resins |
| US20180118645A1 (en) * | 2013-06-13 | 2018-05-03 | Empire Technology Development Llc | Multi-functional phenolic resins |
| CN107987661A (en) * | 2017-12-29 | 2018-05-04 | 西北农林科技大学 | A kind of biomass graphene modified raw lacquer heavy antisepsis composite coating and preparation method thereof |
| CN108659675A (en) * | 2018-05-23 | 2018-10-16 | 中国海洋大学 | A kind of preparation method of the Long-effect corrosion-resistant wave transparent coating of graphene modification silicon nitride |
| CN110499086A (en) * | 2019-07-19 | 2019-11-26 | 武汉理工大学 | A kind of silicon nitride comprising graphene oxide composite granule solventless epoxy coating and the preparation method and application thereof |
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