CN117603619A - Coating containing photo-thermal curing resin and preparation method thereof - Google Patents

Coating containing photo-thermal curing resin and preparation method thereof Download PDF

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Publication number
CN117603619A
CN117603619A CN202311564797.3A CN202311564797A CN117603619A CN 117603619 A CN117603619 A CN 117603619A CN 202311564797 A CN202311564797 A CN 202311564797A CN 117603619 A CN117603619 A CN 117603619A
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photo
photoinitiator
coating
acrylic ester
nano silicon
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谢梦静
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Zheming Printing Ink & Paintings Guangzhou Co ltd
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Zheming Printing Ink & Paintings Guangzhou Co ltd
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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
    • 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
    • C09D5/18—Fireproof paints including high temperature resistant paints
    • 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
    • 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
    • C09D7/63—Additives non-macromolecular organic
    • 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
    • C09D7/65—Additives macromolecular
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00—Properties
    • C08L2201/08—Stabilised against heat, light or radiation or oxydation
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00—Polymer mixtures characterised by other features
    • C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
    • C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Paints Or Removers (AREA)

Abstract

The invention relates to the field of coatings, and particularly discloses a coating containing photo-thermal curing resin and a preparation method thereof. Wherein the coating containing the photo-thermal curing resin comprises the following components: aliphatic urethane acrylates; a urethane acrylate; modified polyurethane acrylic ester containing nano silicon dioxide grafted on the surface; a carbon-accumulating resin; a polyisocyanate; a diluent; a photoinitiator; and (3) a leveling agent. The preparation method of the coating containing the photo-thermal curing resin comprises the following steps: the components are mixed in sequence to obtain the coating containing the photo-thermal curing resin. The coating provided by the invention has the advantages of high toughness, high adhesive force and higher heat resistance; in addition, the preparation method of the invention has the advantages of simplicity, convenience and easy industrial production.

Description

Coating containing photo-thermal curing resin and preparation method thereof
Technical Field
The invention relates to the field of coatings, in particular to a coating containing photo-thermal curing resin and a preparation method thereof.
Background
In recent years, the development of the paint in China is rapid, and various aspects such as the type, the performance and the quality of the paint are greatly improved. Along with the continuous enhancement of environmental protection force of the country, the paint industry is gradually approaching to the green and sustainable development direction at the same time.
In the fields of art decorations, toys and the like, in order to prevent potential hazards to the safety of children caused by the fact that a surface coating is too hard, generally, a water-based polyurethane coating with high flexibility is selected, and the water-based polyurethane coating can be rapidly cured under ultraviolet irradiation, so that the water-based polyurethane coating is an environment-friendly water-based coating with wide application and great potential.
However, even though the photo-curing speed of the aqueous polyurethane coating is high, the aqueous polyurethane coating inevitably has a certain thickness when forming a coating layer, so that the aqueous polyurethane coating placed inside is easy to cause the condition that the aqueous polyurethane coating is difficult to be irradiated by ultraviolet light in the curing process, and the curing speed is easy to be influenced. Therefore, the problem of incomplete ultraviolet curing is solved by combining two technical means of light curing and heat curing in the market. However, since the soft segment in the aqueous polyurethane coating is composed of a polyol and a polyamine, the glass transition temperature is low, the heat resistance is generally poor, and if the aqueous polyurethane coating is directly cured by heat after photo-curing, the coating may be aged to cause cracking and peeling of the surface coating. Thus, there is still room for improvement.
Disclosure of Invention
In order to improve heat resistance while providing excellent flexibility to the coating and enable the water-based coating to realize photo-curing and thermal curing at the same time, the application provides a coating containing photo-curing resin and a preparation method thereof.
In a first aspect, the present application provides a coating containing a photo-thermal curable resin, which adopts the following technical scheme:
a coating containing photo-thermal curing resin comprises the following components in parts by weight:
38-39 parts of aliphatic polyurethane acrylic ester;
25-26 parts of polyurethane acrylic ester;
11-12 parts of modified polyurethane acrylic ester containing nano silicon dioxide grafted on the surface;
5-6 parts of carbon-rich resin;
6-7 parts of polyisocyanate;
7-9 parts of a diluent;
3-4 parts of a photoinitiator;
1-2 parts of leveling agent.
By adopting aliphatic polyurethane acrylate, modified polyurethane acrylate containing nano silicon dioxide grafted on the surface, carbon-rich resin and polyisocyanate as raw materials, the coating can be cured through light curing or heat curing, thereby being beneficial to accelerating the curing speed of the coating and improving the construction efficiency of the coating.
Meanwhile, the aliphatic polyurethane acrylic ester and polyurethane acrylic ester are compounded to serve as raw materials, so that the flexibility and elastic potential energy of the coating are improved, the coating can be firmly attached to the surface of an object, and cracking is not easy to occur. By adding the polyisocyanate, the modified polyurethane acrylate containing the nano silicon dioxide grafted on the surface, and the compounding of the carbon resin, the aliphatic polyurethane acrylate and the polyurethane acrylate, the functions of the internal and external adhesives are fully exerted, the crosslinking density is improved, and a three-dimensional network structure with higher thermal stability is formed, so that the heat resistance of the coating is improved, and the aging and adhesive force reduction phenomena of the coating are not easy to occur due to lower heat resistance of the coating in a heat curing stage; meanwhile, certain water is generated in the paint by compounding the various substances, and the water and the polyisocyanate are polymerized to generate fine carbon dioxide pores in the paint, so that a certain deformation space is provided for the paint under the influence of external thermal expansion and cold contraction, the elasticity of the paint is improved, the flexibility of the paint is not easily reduced greatly due to the increase of the crosslinking density, and the paint has heat resistance and flexibility at the same time; and fine carbon dioxide pores generated in the coating are also beneficial to slowing down heat conduction, so that the heat resistance of the coating is further improved, and the coating is less prone to aging and cracking in the heat curing process.
Preferably, the modification method of the modified polyurethane acrylate containing the surface grafted nano silicon dioxide comprises the following steps: polyvinylpyrrolidone, sodium dodecyl benzene sulfonate, nano silicon dioxide and deionized water (0.03-0.05): (0.02-0.03): (40-50): mixing (800-1000) in mass ratio, stirring at 100-200r/min for 20-30 min, filtering and drying to obtain modified nano silicon dioxide; and then mixing the modified nano silicon oxide with polyurethane acrylic ester (3.5-4.0): (1.0-1.5) to obtain the modified polyurethane acrylic ester containing the surface grafted nano silicon dioxide.
The modified nano silicon dioxide is compounded by adopting the substances with the specific proportion, and the modified polyurethane acrylic ester containing the nano silicon dioxide grafted on the surface is prepared by utilizing the modified silicon dioxide, so that the heat resistance of the coating is improved; meanwhile, the modified polyurethane acrylic ester containing the nano silicon dioxide grafted on the surface is not easy to excessively crosslink with other raw materials, so that the toughness of the coating is reduced.
Preferably, the modified nano silicon oxide and polyurethane acrylate are (3.6-3.9): (1.1-1.4) by mass.
The modified nano silicon oxide and polyurethane acrylic ester with specific proportions are added, so that the heat resistance of the coating is improved, and the flexibility of the coating is not easily affected.
Preferably, the photoinitiator consists of photoinitiator 184 and photoinitiator TPO.
By adopting the substances as the photoinitiator, the method is beneficial to improving the generation rate of free radicals, accelerating the polymerization reaction, strengthening the curing of the coating and preparing the coating with better quality.
Preferably, the photoinitiator is formed by mixing the photoinitiator 184 and the photoinitiator TPO in a mass ratio of (2.5-2.7): 0.8-1.1.
By adopting the substances as the photoinitiator, the crosslinking of the oligomer is enhanced; but also to enhance the thermal stability of the coating.
Preferably, the diluent consists of dipentaerythritol hexaacrylate and diethylene glycol butyl ether acetate.
By adopting the substances as the diluent, the viscosity of the coating system is favorably adjusted, the components are fully contacted, the crosslinking of the oligomer is promoted, and the curing efficiency of the coating is improved.
Preferably, the leveling agent is one or more of Tego 140, tego 270 and Tego 340, and is specifically selected from Tego 140.
By adopting the substances as the leveling agent, the viscosity of the coating is improved, the surface tension of the coating liquid is reduced, the coating forms a smooth and even coating film on the surface of an object, and the softness and glossiness of the coating are improved.
In a second aspect, the present application provides a method for preparing a coating containing a photo-thermosetting resin, which adopts the following technical scheme:
a preparation method of a coating containing photo-thermal curing resin comprises the following specific steps:
mixing aliphatic polyurethane acrylic ester, modified polyurethane acrylic ester containing nano silicon dioxide grafted on the surface, polycarbonate resin, polyisocyanate, diluent, photoinitiator and flatting agent, and uniformly stirring to obtain the coating containing the photo-thermal curing resin.
By adopting the technical scheme, a plurality of substances can be better mutually cooperated and compounded, and the coating with better quality can be prepared.
In summary, the present application has the following beneficial effects:
1. by adding the aliphatic polyurethane acrylic ester and the polyurethane acrylic ester for compounding, the flexibility and the elastic potential energy of the coating are improved, so that the coating can be firmly attached to the surface of an object, and the cracking phenomenon is not easy to occur.
2. The modified polyurethane acrylic ester with the nano silicon dioxide grafted on the surface is compounded by adding the carbon-containing resin, so that the effect of the internal and external adhesives is fully exerted, the crosslinking density is improved, a three-dimensional network structure with higher thermal stability is formed, the heat resistance of the coating is improved, and the phenomenon that the adhesive force is reduced due to lower heat resistance and easy aging of the coating in a heat curing stage is avoided.
3. The polyisocyanate, the modified polyurethane acrylic ester containing the nano silicon dioxide grafted on the surface and the carbon-rich resin are added for compounding, so that fine carbon dioxide pores are generated in the paint, a certain deformation space is provided for the paint under the influence of external thermal expansion and cold contraction, the flexibility of the paint along with the change of external environment is improved, and the flexibility is not easy to be greatly reduced due to the increase of hardness; meanwhile, fine carbon dioxide pores in the coating are beneficial to slowing down heat conduction and improving the high temperature resistance of the coating.
Detailed Description
The present application is described in further detail below with reference to examples.
The following examples and comparative examples were all commercially available and were prepared as follows:
polyurethane acrylic ester is purchased from Taiwan Changxing chemical industry Co., ltd, and the molecular weight (g/mol) is 15000-20000;
aliphatic urethane acrylate is purchased from Taiwan Changxing chemical Co., ltd, and has a molecular weight (g/mol) of 1000;
polyisocyanates were purchased from the company Wuhan Kano technology Co., ltd and numbered 65498-23-9;
nonionic polyacrylamides were purchased from Ming Xiang chemical technology (Shandong) group Co., ltd;
anionic polyacrylamide was purchased from Shanghai festival cleaning chemical Co., ltd;
sodium dodecyl benzene sulfonate was purchased from Shanghai Seiyaka Biotechnology Co., ltd;
dipentaerythritol hexaacrylate was purchased from Jin Jinle chemical company, inc;
photoinitiator 184 was purchased from wuhan's biosciences limited;
the photoinitiator TPO was purchased from Wuhan Fuxin chemical Co., ltd;
the initiator IHT-PI EMK is purchased from Hubei Yongku technology Co., ltd;
photoinitiator IHT-PI MBP was purchased from Shanghai Seiyaka Biotechnology Co., ltd;
tego 140 is available from Changsha high technology Co., ltd;
the CAS number of the carbon polymer resin is 24936-68-3;
the CAS number of the hydrogenated bisphenol A epoxy resin is 30583-72-3;
naphthalene 1, 5-diisocyanate has a CAS number of 3173-72-6;
the CAS number of the nano silicon dioxide is 60676-86-0;
the CAS number of polyvinylpyrrolidone is 9003-39-8;
diethylene glycol butyl ether acetate has a CAS number of 124-17-4.
Preparation example 1
The preparation example of the application discloses a modification method of modified polyurethane acrylic ester containing nano silicon dioxide grafted on the surface, which comprises the following specific steps:
adding 0.03g of polyvinylpyrrolidone, 0.02g of sodium dodecyl benzene sulfonate and 40g of nano silicon dioxide into 800mL of deionized water, stirring at a rotating speed of 100r/min for 30 minutes, filtering by using a funnel, and drying the obtained filter cake in a baking oven at a temperature of 60 ℃ to obtain modified nano silicon dioxide; and adding 3.5g of modified nano silicon oxide and 1.0g of polyurethane acrylate into a container, and stirring at a rotating speed of 100r/min for 30 minutes to obtain the modified polyurethane acrylate containing the surface grafted nano silicon dioxide.
Preparation example 2
The preparation example of the application discloses a modification method of modified polyurethane acrylic ester containing nano silicon dioxide grafted on the surface, which comprises the following specific steps:
adding 0.05g of polyvinylpyrrolidone, 0.03g of sodium dodecyl benzene sulfonate and 50g of nano silicon dioxide into 1000mL of deionized water, stirring at a rotating speed of 200r/min for 20 minutes, filtering by using a funnel, and drying the obtained filter cake in a baking oven at a temperature of 60 ℃ to obtain modified nano silicon dioxide; and adding 4.0g of modified nano silicon oxide and 1.5g of polyurethane acrylate into a container, and stirring at a rotating speed of 200r/min for 20 minutes to obtain the modified polyurethane acrylate containing the surface grafted nano silicon dioxide.
Preparation example 3
The difference from the preparation example 1 is that: the equivalent nonionic polyacrylamide is used for replacing polyvinylpyrrolidone.
Preparation example 4
The difference from the preparation example 1 is that: the sodium dodecyl benzene sulfonate is replaced by equivalent anionic polyacrylamide.
Example 1
The embodiment of the application discloses a coating containing photo-thermal curing resin, which comprises the following components in parts by mass:
38kg of aliphatic urethane acrylate; 25kg of polyurethane acrylate; 11kg of modified polyurethane acrylate containing nano silicon dioxide grafted on the surface; 5kg of a carbon-rich resin; 6kg of polyisocyanate; 9kg of diluent; 4kg of a photoinitiator; 2kg of leveling agent.
In this example, a modified urethane acrylate containing surface grafted nano silica was prepared as in preparation example 1.
The photoinitiator may be any photoinitiator conventional in the art, and in this embodiment, the photoinitiator is defined by photoinitiator 184 and a photoinitiator TPO of 2.5:0.8 mass ratio.
The diluent may be any diluent conventional in the art, and in this embodiment, the diluent is selected from the group consisting of dipentaerythritol hexaacrylate and diethylene glycol butyl ether acetate in a ratio of 1:1, and the mass ratio of the components is 1.
The leveling agent may be any leveling agent conventional in the art, and in this embodiment, tego 140 is specifically selected.
The embodiment of the application also discloses a preparation method of the coating containing the photo-thermal curing resin, which comprises the following steps: adding aliphatic polyurethane acrylic ester, modified polyurethane acrylic ester containing nano silicon dioxide grafted on the surface, polycarbonate resin, polyisocyanate, diluent, photoinitiator and Tego 140 into a container, and stirring at a rotating speed of 50r/min for 30 minutes to obtain the coating containing the photo-thermal curing resin.
Example 2
The difference from example 1 is that: the added mass of each component is different, and the concrete steps are as follows:
39kg of aliphatic urethane acrylate; 26kg of polyurethane acrylate; 12kg of modified polyurethane acrylate containing nano silicon dioxide grafted on the surface; 6kg of a carbon-rich resin; 7kg of polyisocyanate; 7kg of diluent; 3kg of a photoinitiator; 1kg of leveling agent.
In this example, a modified urethane acrylate containing surface grafted nano silica was prepared as in preparation example 2.
The photoinitiator may be any photoinitiator conventional in the art, and in this embodiment, the photoinitiator is defined by photoinitiator 184 and photoinitiator TPO at 2.7: 1.1.
The diluent may be any diluent conventional in the art, and in this embodiment, dipentaerythritol hexaacrylate is specifically selected.
The leveling agent may be any leveling agent conventional in the art, and in this embodiment, tego 270 is specifically selected.
The embodiment of the application also discloses a preparation method of the coating containing the photo-thermal curing resin, which comprises the following steps:
adding aliphatic polyurethane acrylic ester, modified polyurethane acrylic ester containing nano silicon dioxide grafted on the surface, polycarbonate resin, polyisocyanate, dipentaerythritol hexaacrylic ester, photoinitiator and Tego 140 into a container, and stirring at a rotating speed of 50r/min for 30 minutes to obtain the coating containing the photo-thermal curing resin.
Example 3
The difference from example 1 is that: the added mass of each component is different, and the concrete steps are as follows:
38.5kg of aliphatic urethane acrylate; 25.5kg of polyurethane acrylate; 11.5kg of modified polyurethane acrylate containing nano silicon dioxide grafted on the surface; 5.5kg of carbon-rich resin; 6.5kg of polyisocyanate; 8kg of diluent; 3.5kg of photoinitiator; 1.5kg of leveling agent.
The photoinitiator may be any photoinitiator conventional in the art, and in this embodiment, the photoinitiator is defined by photoinitiator 184 and photoinitiator TPO at 2.6:0.95 mass ratio.
Example 4
The difference from example 3 is that:
the photoinitiator is specifically selected from photoinitiator IHT-PI EMK and photoinitiator TPO, and the mass ratio of the photoinitiator IHT-PI EMK to the photoinitiator TPO is 2.5:0.8.
example 5
The difference from example 3 is that:
the photoinitiator is specifically selected from a photoinitiator 184 and a photoinitiator IHT-PI MBP, and the mass ratio of the photoinitiator 184 to the photoinitiator IHT-PI MBP is 2.5:0.8.
example 6
The difference from example 3 is that: the modified polyurethane acrylic ester containing the nano silicon dioxide grafted on the surface is prepared in preparation example 3.
Example 7
The difference from example 3 is that: the modified polyurethane acrylic ester containing the nano silicon dioxide grafted on the surface is prepared in preparation example 4.
Comparative example 1
The comparative example of the present application discloses a coating material containing a photo-thermal curing resin, which comprises the following components by mass:
38.5kg of aliphatic urethane acrylate; 25.5kg of polyurethane acrylate; 8kg of diluent; 3.5kg of photoinitiator; 1.5kg of leveling agent.
The photoinitiator may be any photoinitiator conventional in the art, and in this embodiment, the photoinitiator is defined by photoinitiator 184 and photoinitiator TPO at 2.6:0.95 mass ratio.
The diluent may be any diluent conventional in the art, and in this embodiment, the diluent is selected from the group consisting of dipentaerythritol hexaacrylate and diethylene glycol butyl ether acetate in a ratio of 1:1, and the mass ratio of the components is 1.
The leveling agent may be any leveling agent conventional in the art, and in this embodiment, tego 140 is specifically selected.
The comparative example also discloses a preparation method of the coating containing the photo-thermal curing resin, which comprises the following specific steps:
adding aliphatic polyurethane acrylic ester, a diluent, a photoinitiator and Tego 140 into a container, and stirring for 30 minutes at a rotating speed of 50r/min in a dark place to obtain the coating containing the photo-thermal curing resin.
Comparative example 2
The difference from example 3 is that: the polycarbonate resin was replaced with an equivalent amount of hydrogenated bisphenol a epoxy resin.
Comparative example 3
The difference from example 3 is that: the modified polyurethane acrylic ester containing the nano silicon dioxide grafted on the surface is replaced by the polyurethane acrylic ester with the same amount.
Comparative example 4
The difference in example 3 is that: the polyisocyanate was replaced with an equivalent amount of naphthalene 1, 5-diisocyanate.
Experiment 1
Preparation of paint film samples: the paint prepared in the above examples and comparative examples is used, and GB912 common carbon steel plates with the length, width and thickness of 120mm and 50mm and 0.45mm are fixed on a putty knife coater, and are painted on a specified test plate by a paint brush for 3 times in the longitudinal and transverse directions, so that a layer of uniform paint is formed, and blank or overflow phenomenon cannot occur. Then the steel plate coated with the coating is placed on an LED-UV double-layer curing box with the weight of 250mW/cm 2 Is irradiated for 5 minutes; and then transferring to an oven with the temperature of 72 ℃ for drying at high temperature for 30 minutes to obtain a paint film sample. Wherein the LED-UV dual layer curing box is purchased from Bangwo electronic technologies Inc. of Guangzhou. And the following tests were carried out on paint film samples:
detection 1
The prepared paint films were taken out respectively, the surface state of the paint films after heat curing was observed, and the results were recorded.
Detection 2
The prepared paint film samples are respectively taken for flexibility test according to GB/T1731-2020 paint film and putty film flexibility test method, each group of examples and preparation examples are respectively tested for three times, and the average value is obtained. Wherein, the paint film flexibility tester is purchased from Mo Jiangan Mei precision instrument in Dongguan city.
Detection 3
The prepared paint film samples are respectively taken, pencil hardness test is carried out on the paint according to the A method-testing machine method in GB/T6739-1966 pencil test method for coating hardness, each group of examples and preparation examples are respectively tested three times, and average value is obtained. Wherein the pencil hardness tester used was purchased from Lyte instruments Inc. of Shenzhen city.
Detection 4
The RCA paper tape wear-resistant testing machine is placed on a horizontal tabletop, and four foot pads of the instrument are adjusted to enable the level to be placed in the central position, so that the RCA paper tape wear-resistant testing machine is in a horizontal state. A weight with the mass of 175g is selected to be fixed on an RCA paper tape wear-resistant tester, the prepared paint film samples are respectively taken to be fixed under a grinding head of the RCA paper tape wear-resistant tester, a sliding bolt and a swinging arm are adjusted by aligning the grinding positions with the selected test points, the instrument is started, the wear condition of a paint film is observed after 5 revolutions is tested, the revolution of the paint film when the paint film is worn through is recorded, and the average value is obtained after 3 repeated tests. RCA paper tape abrasion resistance testing machine was purchased from Shanghai celebration equipment limited.
Detection 5
The prepared paint film samples are respectively taken, a heat resistance experiment is carried out on the paint according to the step 6 in GB/T1735-2009 test of heat resistance of colored paint and varnish, and the heat resistance of the paint is evaluated from the aspects of glossiness, adhesive force and water boiling adhesive force.
Gloss level: 3 of the above-prepared panels were used for each of the examples and comparative examples, and the gloss of a paint film was measured at 60℃by referring to GB1743-1979 paint film gloss assay, and the average value was taken. Gloss detectors were purchased from Sanhen technologies Inc.
Adhesion force: each set of examples and comparative examples were tested for adhesion by taking 3 of the above prepared templates, respectively, and by referring to test method a in astm d 3359.
Boiling power: 2L of deionized water is heated and kept at 100 ℃, 3 templates of each group of examples and comparative examples are respectively and correspondingly immersed in hot water completely, the templates are taken out after being boiled for 120min, the templates are stood at normal temperature and cooled to room temperature, whether the surface of a sample coating is abnormal or not is checked, paint film graining is carried out according to the GB/T9286-98 standard, grading is carried out according to the implementation results and the experimental results are recorded.
TABLE 1
The experimental detection data are shown in Table 2.
TABLE 2
According to the data of the example 3 and the comparative example 1 in the table 2, the addition of the aliphatic urethane acrylate and the urethane acrylate in the comparative example 1 is favorable for forming the coating with higher flexibility, but the heat resistance of the coating is poor at the same time, the aging of the paint film is easy to cause the crack of the paint film after the heat curing, and the surface of the paint film is dull and dull; reduced flexibility, hardness and wear resistance; after the heat resistance test, the gloss and adhesion of the paint film are reduced. Example 3 the addition of the surface grafted nano silica, the polycarbonic resin and the polyisocyanate on the basis of comparative example 1 improves the heat resistance of the coating and has better flexibility. The embodiment is proved to be added with aliphatic polyurethane acrylic ester, surface grafting nano silicon dioxide, carbon-rich resin and polyisocyanate for synergistic compounding, thereby being beneficial to improving the heat resistance of the coating and not affecting the flexibility of the coating.
From the comparison of the data of example 3 and comparative examples 2 to 4 in Table 2, no cracks and no moire occurred in example 3, and the gloss of the panel after the aging test was 80.3 and the adhesion was 4B; comparative examples 2 to 4 respectively replaced the surface grafted nano silica, the polycarbonate resin and the polyisocyanate with the same amount of hydrogenated bisphenol A epoxy resin, polyurethane acrylate and 1, 5-naphthalene diisocyanate, and the surface glossiness of the coating after heat curing was reduced; performing a flexibility test, wherein the coating is provided with a net crack and a net curve; and after the ageing test, the gloss and adhesion of the panels were much lower than in example 3. The modified polyurethane acrylic ester containing nano silicon dioxide grafted on the surface and the polyisocyanate are added to compound, so that the effect of the internal and external adhesives is fully exerted, the crosslinking density is improved, a three-dimensional network structure with higher thermal stability is formed, the heat resistance of the coating is improved, and the phenomena of ageing and reduced glossiness of the coating due to lower heat resistance in a heat curing stage are avoided. Only if the aliphatic polyurethane acrylate, polyurethane acrylate carbon resin, modified polyurethane acrylate containing nano silicon dioxide grafted on the surface, carbon resin and polyisocyanate are added for compounding, the heat resistance of the coating is improved, the flexibility of the coating is not affected, and one of the substances is replaced at will, so that the effect cannot be achieved.
From the comparison of the data in examples 3-5 of Table 2, example 3 uses a specific type of photoinitiator, which is advantageous in improving the initiation efficiency of the resin, enhancing the heat resistance of the coating, and at the same time not easily affecting the flexibility of the coating.
According to the data comparison of example 3 and examples 6-7 in Table 2, modified polyurethane acrylate is prepared by using polyvinyl pyrrolidone and sodium dodecyl benzene sulfonate modified nano silicon dioxide in specific proportion and polyurethane acrylate, which is beneficial to improving the heat resistance of the coating and does not affect the flexibility of the coating.
The present embodiment is merely illustrative of the present application and is not intended to be limiting, and those skilled in the art, after having read the present specification, may make modifications to the present embodiment without creative contribution as required, but is protected by patent laws within the scope of the claims of the present application.

Claims (8)

1. A coating material containing a photo-curable resin, characterized in that: comprises the following components in parts by mass:
38-39 parts of aliphatic polyurethane acrylic ester;
25-26 parts of polyurethane acrylic ester;
11-12 parts of modified polyurethane acrylic ester containing nano silicon dioxide grafted on the surface;
5-6 parts of carbon-rich resin;
6-7 parts of polyisocyanate;
7-9 parts of a diluent;
3-4 parts of a photoinitiator;
1-2 parts of leveling agent.
2. A coating material containing a photo-thermosetting resin according to claim 1, wherein: the modification method of the modified polyurethane acrylic ester containing the nano silicon dioxide grafted on the surface comprises the following steps: polyvinylpyrrolidone, sodium dodecyl benzene sulfonate, nano silicon dioxide and deionized water (0.03-0.05): (0.02-0.03): (40-50): mixing (800-1000) in mass ratio, stirring at 100-200r/min for 20-30 min, filtering and drying to obtain modified nano silicon dioxide; and then mixing the modified nano silicon dioxide with polyurethane acrylic ester (3.5-4.0): (1.0-1.5) to obtain the modified polyurethane acrylic ester containing the surface grafted nano silicon dioxide.
3. A coating material containing a photo-thermosetting resin according to claim 2, wherein: the modified nano silicon oxide and polyurethane acrylic ester are (3.6-3.9): (1.1-1.4) by mass.
4. A coating material containing a photo-thermosetting resin according to claim 1, wherein: the photoinitiator consists of photoinitiator 184 and photoinitiator TPO.
5. A coating material containing a photo-setting resin as claimed in claim 4, wherein: the photoinitiator consists of a photoinitiator 184 and a photoinitiator TPO in a mass ratio of (2.5-2.7): (0.8-1.1).
6. A coating material containing a photo-thermosetting resin according to claim 1, wherein: the diluent consists of dipentaerythritol hexaacrylate and diethylene glycol butyl ether acetate.
7. A coating material containing a photo-thermosetting resin according to claim 1, wherein: the leveling agent is one or more of Tego 140, tego 270 and Tego 340.
8. A method for producing a coating material containing a photo-thermosetting resin as claimed in any one of claims 1 to 7, characterized in that: the specific operation is as follows:
mixing aliphatic polyurethane acrylic ester, modified polyurethane acrylic ester containing nano silicon dioxide grafted on the surface, polycarbonate resin, polyisocyanate, diluent, photoinitiator and flatting agent, and uniformly stirring to obtain the coating containing the photo-thermal curing resin.
CN202311564797.3A 2023-11-22 2023-11-22 Coating containing photo-thermal curing resin and preparation method thereof Pending CN117603619A (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104403550A (en) * 2014-11-03 2015-03-11 深圳市千浪化工有限公司 Free-radical chain polymerization thinly-coated ultraviolet-cured nanometer paint
CN110669427A (en) * 2019-11-07 2020-01-10 三河亮克威泽工业涂料有限公司 Two-component water-based UV coating, preparation method and application thereof, and coating piece
CN113717631A (en) * 2021-01-27 2021-11-30 浙江佑谦特种材料有限公司 Water-based UV coating and preparation method and application thereof
CN113773440A (en) * 2021-10-12 2021-12-10 中国石油大学(华东) Water-based drilling fluid filtrate reducer capable of inhibiting natural gas hydrate decomposition and preparation method and application thereof
CN116200073A (en) * 2023-03-10 2023-06-02 广州市哲铭油墨涂料有限公司 Water-based ink with quick-drying function and preparation method thereof

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104403550A (en) * 2014-11-03 2015-03-11 深圳市千浪化工有限公司 Free-radical chain polymerization thinly-coated ultraviolet-cured nanometer paint
CN110669427A (en) * 2019-11-07 2020-01-10 三河亮克威泽工业涂料有限公司 Two-component water-based UV coating, preparation method and application thereof, and coating piece
CN113717631A (en) * 2021-01-27 2021-11-30 浙江佑谦特种材料有限公司 Water-based UV coating and preparation method and application thereof
CN113773440A (en) * 2021-10-12 2021-12-10 中国石油大学(华东) Water-based drilling fluid filtrate reducer capable of inhibiting natural gas hydrate decomposition and preparation method and application thereof
CN116200073A (en) * 2023-03-10 2023-06-02 广州市哲铭油墨涂料有限公司 Water-based ink with quick-drying function and preparation method thereof

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