CN114958188A - Thermochromic water-based UV coating and preparation method thereof - Google Patents
Thermochromic water-based UV coating and preparation method thereof Download PDFInfo
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- CN114958188A CN114958188A CN202210607057.2A CN202210607057A CN114958188A CN 114958188 A CN114958188 A CN 114958188A CN 202210607057 A CN202210607057 A CN 202210607057A CN 114958188 A CN114958188 A CN 114958188A
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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
- C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
- C09D175/04—Polyurethanes
- C09D175/14—Polyurethanes having carbon-to-carbon unsaturated bonds
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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
- 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
- C09D183/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
- C09D183/04—Polysiloxanes
- C09D183/08—Polysiloxanes containing silicon bound to organic groups containing atoms other than carbon, hydrogen, and oxygen
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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
- C09D5/26—Thermosensitive 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
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2258—Oxides; Hydroxides of metals of tungsten
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2265—Oxides; Hydroxides of metals of iron
- C08K2003/2272—Ferric oxide (Fe2O3)
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
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- Paints Or Removers (AREA)
Abstract
The invention provides a thermochromic water-based UV coating and a preparation method thereof, and is characterized in that the coating is prepared from the following raw materials in parts by weight: 20-50 parts of carboxyl modified water-soluble polyurethane acrylate, 10-20 parts of bisphenol A epoxy resin, 10-20 parts of organic silicon modified acrylate, 0.6-3 parts of high-temperature resistant color-changing pigment, 10-30 parts of active diluent, 0.2-1 part of defoaming agent, 3-10 parts of photoinitiator and 6-15 parts of curing agent. The carboxyl modified water-soluble polyurethane acrylate is adopted, has high functionality, strong polarity and high strength, can be used in photocureable coating, can reduce the using amount of reactive diluent, has high curing speed, good adhesive film flexibility and strong adhesive force, and has excellent adhesive force to polar substrates such as wood; the organosilicon modified acrylate main chain is a silicon-oxygen bond, so that the flexibility of the coating can be effectively improved, and the water resistance and the hot adhesion resistance of the coating are improved.
Description
Technical Field
The invention relates to the technical field of wood floors, in particular to a thermochromic aqueous UV coating and a preparation method thereof.
Background
In order to improve the visual effect and the texture of the solid wood floor, protect the base material and prolong the service life of the floor, a paint film with high hardness, high wear resistance, scratch resistance, easy cleaning and high smoothness is formed on the surface layer of the floor by coating paint on the surface, so that the dimension of the floor can be kept stable for a long time, and the service life of the floor is prolonged.
However, when the solid wood floor is in an environment with large temperature and humidity changes (such as a geothermal environment), the surface of the solid wood floor cracks due to the different adaptability of the paint film and the base material to the deformation, which affects the appearance quality and the service life of the floor.
The water-based paint is a paint taking water as a dispersion medium or a solvent, and has attracted wide attention due to the characteristics of low VOC, energy conservation and environmental protection. The water-based paint is applied to the fields of furniture, wood doors and the like, but is not well applied to floors. The breakthrough of the application of the water-based paint on the wood floor is realized, and the following problems need to be solved: 1) the solid content of the water-based paint is low, the filling property is general, and the closed coating effect is not ideal enough; 2) the hardness of a paint film of the water-based paint is difficult to meet the standard requirement of paint decoration of the wooden floor, and certain gaps also exist in the performances such as fullness, pollution resistance and the like; 3) the surface tension of water in the water-based paint is large, the volatilization speed of the water-based paint is not as fast as that of a common organic solvent, so that the paint surface film forming speed of the water-based paint is slow, and the production efficiency of a water-based paint production line is lower than that of an oil-based paint production line. For the above reasons, the water-based paint has not been well popularized on wood floors. However, due to the stricter environmental policy and the stricter VOC restriction standard of coating materials, the problem of changing oil into water in wood floor coating is urgently solved.
Meanwhile, with the rise of the home decoration industry, people pay more and more attention to the style of indoor decoration design, and the floor decoration is also required to meet the requirements of consumers as a main part of the decoration. At the present stage, although the types of the floor boards are many, the floor boards are single, cannot reflect personalized differences, and cannot meet the requirements of part of people on pursuing fashion and showing self.
Disclosure of Invention
In view of the above, the present invention aims to provide a thermochromic aqueous UV coating and a preparation method thereof.
The technical scheme of the invention is as follows:
the thermochromic water-based UV coating for coating the wood floor is prepared from the following raw materials in parts by weight:
the high-temperature resistant color-changing pigment is a graphene-loaded tungsten trioxide/ferric oxide nano material, and the preparation method comprises the following steps:
dispersing 0.1-0.8 part of ferrous nitrate and 0.7-1.8 parts of ferrous tungstate into 20-40 parts of 0.5-1.0M citric acid aqueous solution according to the mass parts, adding 2-8 parts of graphene nano powder, and then controlling the temperature to be 50-70 ℃, stirring and dispersing for 30-60 min; then cooling to room temperature, uniformly mixing 0.05-0.25 part of isopropyl triisostearate and 0.04-0.15 part of acetylacetone amine, adding into a reaction kettle, heating to 60-80 ℃, stirring for reaction for 20-30min, transferring into a hydrothermal kettle after the reaction is finished, controlling the temperature to be 120-800 ℃, reacting for 5-10h, filtering after the reaction is finished, drying, calcining at the temperature of 600-800 ℃ in the atmosphere of air for 3-8h, and finally crushing to nano level to obtain the high temperature resistant color-changing pigment.
Wherein, when the preparation discolours the pigment, this application adopts weak acid material citric acid, rather than the medium and strong acid oxalic acid among the prior art, because oxalic acid can influence the cross-linking reaction, and then influences the stability that discolours the pigment.
The preparation method of the organic silicon modified acrylate comprises the following steps:
A. mixing toluene diisocyanate and dibutyltin dilaurate in a molar ratio of 1:0.01, adding the mixture into a reaction kettle, heating to 40-50 ℃, then dropwise adding pentaerythritol triacrylate containing p-hydroxyanisole serving as a polymerization inhibitor, and reacting at 40-50 ℃ for 4-6 h;
B. and dropwise adding dialkyl silicone oil, continuously heating to 70-75 ℃, testing a reaction product through a Fourier infrared spectrogram until-NCO reaction is complete, and stopping the reaction to obtain the photocuring organic silicon acrylate.
The polymerization inhibitor in the step A comprises p-hydroxyanisole, and the molar ratio of-NCO to-OH in the step A is 2: 1; the molar ratio of-NCO to-OH in step B is less than 1: 1.
The epoxy resin is bisphenol A epoxy resin.
The reactive diluent comprises isobornyl acrylate (IBOA) or 1, 6-hexanediol diacrylate.
The defoaming agent comprises sodium nonyl phenol polyether amine alkyl sulfonate or ethylene-based bis stearamide.
The photoinitiator comprises benzophenone or ethyl N, N-dimethylbenzoate.
The preparation method of the thermochromic water-based UV coating comprises the following steps:
baking the carboxyl modified water-soluble polyurethane acrylate, the organic silicon modified acrylate and the epoxy resin in an oven at 50-60 ℃ for 6-8h, then proportionally adding the above substances and an active diluent into a reaction kettle, dispersing at the rotating speed of 500-600r/min for 1-2h, reducing the rotating speed to 200-300r/min, proportionally adding a curing agent, a photoinitiator, a defoaming agent and a high-temperature-resistant color-changing pigment into the reaction kettle, and dispersing for 0.5-1 h to obtain the water-based UV finish paint.
The application of the temperature-sensitive color-changing water-based UV coating in the coating of the wood floor also belongs to the protection scope of the invention.
Compared with the prior art, the invention has the following beneficial effects:
(1) the carboxyl modified water-soluble polyurethane acrylate is adopted, has high functionality, strong polarity and high strength, can be used in photocureable coating, can reduce the using amount of reactive diluent, has high curing speed, good adhesive film flexibility and strong adhesive force, and has excellent adhesive force to polar base materials such as wood;
(2) the organosilicon modified acrylate main chain is a silicon-oxygen bond, so that the flexibility of the coating can be effectively improved, and the water resistance and the hot adhesion resistance of the coating are improved;
(3) when the color-changing pigment is manufactured, a weakly acidic substance citric acid is adopted in the method, instead of a medium-strong acid oxalic acid in the prior art, because the oxalic acid can influence the cross-linking reaction, the stability of the color-changing pigment is further influenced.
Detailed Description
The present invention will be described in detail with reference to examples. The following examples will aid those skilled in the art in further understanding the present invention, but are not intended to limit the invention in any manner. It should be noted that it would be apparent to those skilled in the art that several modifications and improvements can be made without departing from the inventive concept. All falling within the scope of the present invention.
First, preparation example
Preparation example 1 preparation of high temperature resistant discoloration pigment
Dispersing 0.3 part of ferrous nitrate and 1.5 parts of ferrous tungstate in 30 parts of 1.0M citric acid aqueous solution, adding 5 parts of graphene nano powder, and then controlling the temperature to be 70 ℃, stirring and dispersing for 60 min; and then cooling to room temperature, uniformly mixing 0.25 part of isopropyl triisostearate and 0.1 part of acetylacetone amine, adding the mixture into a reaction kettle, heating to 80 ℃, stirring for reaction for 30min, transferring the mixture into a hydrothermal kettle after the reaction is finished, controlling the temperature to be 120-150 ℃, reacting for 10h, filtering after the reaction is finished, drying, calcining for 3-8h at 800 ℃ in the air atmosphere, and finally crushing to be nano-scale to prepare the high-temperature-resistant color-changing pigment.
Comparative preparation example 1
The difference from preparation example 1 is that citric acid was replaced with oxalic acid.
Preparation example 2 preparation of Silicone-modified acrylate
A. Toluene diisocyanate and dibutyltin dilaurate are mixed and added into a reaction kettle according to the molar ratio of 1:0.01, the temperature is raised to 40 ℃, then pentaerythritol triacrylate containing p-hydroxyanisole as a polymerization inhibitor is added dropwise (the molar ratio of-NCO: -OH is ensured to be 2:1), and the reaction is carried out for 4 hours at 40 ℃;
B. dropwise adding a certain amount of dialkyl silicone oil (-NCO: OH molar ratio is 1:1), continuously heating to 70-75 ℃, testing a reaction product through a Fourier infrared spectrogram until-NCO reaction is complete, and stopping the reaction to obtain the photocuring organic silicon acrylate.
Second, example
Examples 1 to 3
1. Preparing the components and the dosage according to the table 1, and preparing the thermochromic water-based UV coating.
TABLE 1 (Unit: parts by weight)
The preparation method of the thermochromic water-based UV coating comprises the following steps:
according to the formula shown in the table 1, the carboxyl modified water-soluble polyurethane acrylate, the organic silicon modified acrylate and the bisphenol A epoxy resin are dried in an oven at 50-60 ℃ for 6-8h, the resin mixture and the active diluent are added into a reaction kettle according to the proportion, the mixture is dispersed for 1-2h at the rotating speed of 600r/min, the rotating speed is reduced to 300r/min, and the curing agent, the photoinitiator, the defoaming agent and the high-temperature resistant color-changing pigment are added into the reaction kettle according to the proportion and dispersed for 0.5h, so that the water-based UV finish paint is obtained.
Comparative example 1
The difference from example 1 is that: replacing carboxyl modified water-soluble polyurethane acrylate with polybutadiene polyurethane acrylate.
Comparative example 2
The difference from example 1 is that: no silicone modified acrylate was added.
Comparative example 3
The difference from example 1 is that: the high-temperature resistant color-changing pigment is prepared by the pigment prepared in the comparative preparation example 1.
Performance test example 1
The coatings prepared in examples 1-3 and comparative examples 1-3 were heated to remove water and UV cured (cured by a 100-150 ℃ UV lamp for 10-20 seconds and then dried) to obtain paint films.
The test results are shown in Table 2. As can be seen from Table 2, the examples of the present invention have significantly improved solid content, significantly shortened curing time, significantly improved pencil hardness, significantly improved water and weather resistance, and better adhesion and abrasion resistance than the comparative examples.
TABLE 2
The foregoing description has described specific embodiments of the present invention. It is to be understood that the present invention is not limited to the specific embodiments described above, and that various changes and modifications may be made by one skilled in the art within the scope of the appended claims without departing from the spirit of the invention.
Claims (10)
1. The temperature-sensitive color-changing water-based UV coating is characterized by being prepared from the following raw materials in parts by weight:
2. the thermochromic aqueous UV coating according to claim 1, wherein the high-temperature-resistant color-changing pigment is a graphene-loaded tungsten trioxide/ferric oxide nanomaterial, and the preparation method comprises the following steps:
dispersing 0.1-0.8 part of ferrous nitrate and 0.7-1.8 parts of ferrous tungstate into 20-40 parts of 0.5-1.0M citric acid aqueous solution according to the mass parts, adding 2-8 parts of graphene nano powder, and then controlling the temperature to be 50-70 ℃, stirring and dispersing for 30-60 min; then cooling to room temperature, uniformly mixing 0.05-0.25 part of isopropyl triisostearate and 0.04-0.15 part of acetylacetone amine, adding into a reaction kettle, heating to 60-80 ℃, stirring for reaction for 20-30min, transferring into a hydrothermal kettle after the reaction is finished, controlling the temperature to be 120-800 ℃, reacting for 5-10h, filtering after the reaction is finished, drying, calcining at the temperature of 600-800 ℃ in the atmosphere of air for 3-8h, and finally crushing to nano level to obtain the high temperature resistant color-changing pigment.
3. The thermochromic aqueous UV coating according to claim 1, wherein the method for preparing the silicone-modified acrylate comprises the steps of:
A. mixing toluene diisocyanate and dibutyltin dilaurate in a molar ratio of 1:0.01, adding the mixture into a reaction kettle, heating to 40-50 ℃, then dropwise adding pentaerythritol triacrylate containing p-hydroxyanisole serving as a polymerization inhibitor, and reacting at 40-50 ℃ for 4-6 h;
B. and dropwise adding dialkyl silicone oil, continuously heating to 70-75 ℃, testing a reaction product through a Fourier infrared spectrogram until-NCO reaction is complete, and stopping the reaction to obtain the photocuring organic silicon acrylate.
4. The thermochromic aqueous UV coating of claim 3, wherein the polymerization inhibitor in step A comprises p-hydroxyanisole, and the molar ratio of-NCO to-OH in step A is 2: 1; the molar ratio of-NCO to-OH in step B is less than 1: 1.
5. The thermochromic aqueous UV coating of claim 1, wherein the epoxy resin is a bisphenol a epoxy resin.
6. The thermochromic aqueous UV coating of claim 1, wherein the reactive diluent comprises isobornyl acrylate (IBOA) or 1, 6-hexanediol diacrylate.
7. The thermochromic aqueous UV coating of claim 1 wherein the defoamer comprises sodium nonylphenol polyetheramine alkylsulfonate or ethylene bis stearamide.
8. The thermochromic aqueous UV coating of claim 1 wherein the photoinitiator comprises benzophenone or ethyl N, N-dimethylbenzoate.
9. The thermochromic aqueous UV paint of claim 1, wherein the preparation method of the thermochromic aqueous UV paint comprises the following steps:
baking the carboxyl modified water-soluble polyurethane acrylate, the organic silicon modified acrylate and the bisphenol A epoxy resin in an oven at 50-60 ℃ for 6-8h, then proportionally adding the above substances and the active diluent into a reaction kettle, dispersing at the rotating speed of 500-600r/min for 1-2h, reducing the rotating speed to 200-300r/min, proportionally adding the photoinitiator, the defoaming agent and the high-temperature resistant color-changing pigment into the reaction kettle, and dispersing for 0.5-1 h to obtain the water-based UV finish paint.
10. Use of the thermochromic aqueous UV coating according to any of claims 1-9 in the finishing of wood floors.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117210117A (en) * | 2023-10-11 | 2023-12-12 | 全椒亮克威泽工业涂料有限公司 | High-toughness dual-curing UV (ultraviolet) coating and preparation device thereof |
| CN117210117B (en) * | 2023-10-11 | 2024-04-19 | 全椒亮克威泽工业涂料有限公司 | High-toughness dual-curing UV (ultraviolet) coating and preparation device thereof |
| CN117946584A (en) * | 2024-02-19 | 2024-04-30 | 湖南泰利恒友科技开发有限公司 | Laser anti-counterfeiting coating, preparation method thereof and laser transfer film |
| CN117946584B (en) * | 2024-02-19 | 2024-07-19 | 湖南泰利恒友科技开发有限公司 | Laser anti-counterfeiting coating, preparation method thereof and laser transfer film |
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| CN114958188B (en) | 2023-06-06 |
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