CN107715811B - Self-repairing microcapsule for aqueous coating on surface of wood material and preparation method thereof - Google Patents
Self-repairing microcapsule for aqueous coating on surface of wood material and preparation method thereof Download PDFInfo
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- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
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- C08G12/10—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes with acyclic or carbocyclic compounds with acyclic compounds having the moiety X=C(—N<)2 in which X is O, S or —N
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Abstract
The invention relates to a self-repairing microcapsule of a water-based coating on a wood material surface, which comprises the following raw materials in parts by weight: 15-30 parts of urea, 30-50 parts of formaldehyde, 10-20 parts of diethanolamine, 1-5 parts of fluororesin, 3-8 parts of epoxy resin, 7-16 parts of water-based acrylic resin, 0.1-2 parts of photoinitiator, 0.005-2 parts of sodium dodecyl benzene sulfonate and 5-20 parts of distilled water. The invention takes urea and formaldehyde as raw materials of the capsule wall, adds fluororesin and epoxy resin to prepare a modified wall material, takes water-based acrylic resin as a capsule core to prepare a modified polyurea formaldehyde-coated water-based acrylic resin microcapsule, and synthesizes a material with a self-repairing function by using a microcapsule technology.
Description
Technical Field
The invention relates to the field of coatings, in particular to a self-repairing microcapsule of a water-based coating on the surface of a wood material and a preparation method thereof.
Background
At present, the water-based paint is widely applied in the field of wood paint due to the advantages of environmental protection and easy production, but cracks are easy to appear in the using process. Coating, as an important step in adjusting the surface properties of wood materials, has become a key technology in the manufacture and processing of wood products. Through a large amount of research by scholars at home and abroad, the synthesis of the self-repairing material by utilizing the microcapsule technology is possible and has great significance. If the microcapsule is used for self-repairing and applied to the water-based paint, the microcapsule can release a core material healing agent when the wall material of the microcapsule is broken, and the healing agent can generate polymerization reaction or directly act after meeting an exciting agent pre-buried in the water-based paint, so that cracks are bonded, and the utilization and safety of a paint film can be improved.
Disclosure of Invention
The invention aims to solve the problems that cracks are easy to appear in the existing water-based paint in the using process and the quality of other wood surface coating films is high, and provides a wood material surface water-based paint self-repairing microcapsule which has self-repairing performance and can effectively repair the cracks appearing in the using process of the water-based paint on the surfaces of wood products.
Technical scheme
A self-repairing microcapsule of a water-based coating on a wooden material surface comprises the following raw materials in parts by weight:
15-30 parts of urea, 30-50 parts of formaldehyde, 10-20 parts of diethanolamine, 1-5 parts of fluororesin, 3-8 parts of epoxy resin, 7-16 parts of water-based acrylic resin, 0.1-2 parts of photoinitiator, 0.005-2 parts of sodium dodecyl benzene sulfonate and 5-20 parts of distilled water.
The preferable scheme is that the material comprises the following raw materials in parts by weight: 18-25 parts of urea, 35-45 parts of formaldehyde, 12-18 parts of diethanolamine, 2-4 parts of fluororesin, 3.5-7 parts of epoxy resin, 8-15 parts of water-based acrylic resin, 0.4-1.5 parts of photoinitiator, 0.3-1.5 parts of sodium dodecyl benzene sulfonate and 7-18 parts of distilled water.
The photoinitiator is benzoin methyl ether.
The fluororesin can increase the surface hydrophobicity of the wood, thereby reducing the moisture expansion, drying, shrinkage, warping and deformation of the wood due to water absorption, reducing the cracking phenomenon of the coating, enhancing the corrosion resistance of the interface of the water-based coating/wood material and prolonging the service life of the coating. The water-based coating which takes the water-based coating as a film forming substance can dissolve an organic solvent, is cured into a film at normal temperature or high temperature, and can be applied to corrosion prevention of the interface of wood and the water-based coating.
The epoxy resin can enhance the elasticity of the coating, so that the coating has higher compressive strength and is not easy to crack, thereby prolonging the service life of the water-based coating on the surface of the wood.
The preparation method of the self-repairing microcapsule of the water-based paint on the surface of the wood material comprises the following steps:
(1) adding urea into formaldehyde, fully stirring until the urea is dissolved, and adjusting the pH value to 9.0 by using diethanolamine;
(2) adding fluororesin and epoxy resin, fully stirring, adding a magnetic stirrer, uniformly stirring in a constant-temperature water bath at 70 ℃ to obtain a modified urea formaldehyde prepolymer solution, and rapidly cooling to room temperature for later use;
(3) adding sodium dodecyl benzene sulfonate into distilled water, stirring until the sodium dodecyl benzene sulfonate is completely dissolved to obtain a sodium dodecyl benzene sulfonate aqueous solution serving as an emulsifier;
(4) adding a sodium dodecyl benzene sulfonate aqueous solution and a photoinitiator into the water-based acrylic resin, adding a magnetic stirrer for stirring, and stirring and emulsifying in a water bath at 60 ℃ to obtain a stable core material emulsion;
(5) slowly dripping the modified urea formaldehyde prepolymer solution into the core material emulsion at the rotating speed of 300r/min, gradually adding citric acid crystals to adjust the pH to be 2.5-3.0, slowly heating to 65-75 ℃ to react, and then carrying out suction filtration and drying on the obtained product to obtain powder, namely the self-repairing microcapsule of the water-based coating on the surface of the wood material.
Further, in the step (4), the stirring speed of the magnetic stirrer is 1200r/min, and the emulsifying time is 30 min.
Further, in the step (5), the drying temperature is 80 ℃ and the time is 3-5 h.
The invention has the advantages that: the microcapsule method belongs to embedded self-repairing, namely, the repairing agent is embedded in the polymer matrix composite material in the modes of hollow pipelines, capsules and the like, the hollow pipelines and the capsules are broken under the external action, the repairing agent is released to the surfaces of cracks under the action of capillary tubes and generates polymerization reaction with a catalyst in the interface of a wood water-based coating, and therefore the cracks are bonded, and the crack damage is repaired. The fluororesin and the epoxy resin are added into the urea resin to prepare the modified wall material, so that the fluororesin can increase the surface hydrophobicity of the wood, thereby reducing the wet expansion, drying, shrinkage, warping and deformation of the wood due to water absorption, reducing the cracking phenomenon of the coating, enhancing the corrosion resistance of the interface of the water-based coating/wood material and prolonging the service life of the coating; the epoxy resin can enhance the elasticity of the coating, so that the coating has higher compressive strength and is not easy to crack, thereby prolonging the service life of the water-based coating on the surface of the wood, and the wall material is prepared by introducing the fluororesin and the epoxy so that the coating has higher performance. The core material is prepared from water-based acrylic resin and a photoinitiator, and the reaction capsule is broken under the action of the photoinitiator to repair the surface damage of the wood. When the coating is coated on the surface of a wooden product to be used as finish paint, the photocuring rate is high, and the antibacterial and bacteriostatic effects are good.
The invention mainly uses the experiment of microcapsule modified water paint to make the coating have low glossiness, wear resistance, impact resistance and self-repairing capability. The addition amount of the microcapsule in the wood material surface water-based paint is 5-15%, after the microcapsule is added, the glossiness of a coating film is matte, the wear resistance of the coating film is 1 grade (the wear revolution is 5000 turns) according to the national standard GB/T3324-2008, the impact resistance is 50 Kg-cm, and the repair efficiency of the coating is higher than 90%.
Detailed Description
The present invention will be further described with reference to the following specific examples. For comparison, in the following examples, the fluororesin used was a normal temperature self-crosslinking fluorocarbon resin produced by Nanjing New-Seiko chemical engineering Co., Ltd, the epoxy resin used was a bisphenol-based propane epoxy resin produced by Wuxi city Changcheng chemical engineering Co., Ltd, and the aqueous acrylic resin used was an aqueous acrylic resin GS-356 produced by Changzhou Guangzhou chemical engineering Co., Ltd, but not limited thereto.
Example 1
(1) Adding 18g of urea and 33g of formaldehyde into a beaker, fully stirring until the urea is dissolved, and adjusting the pH value to about 9.0 by using 12g of diethanolamine;
(2) adding 3g of fluororesin and 5g of epoxy resin, fully stirring, adding a magnetic stirrer, stirring for 1h in a constant-temperature water bath at 70 ℃ to obtain slightly viscous transparent modified urea formaldehyde prepolymer solution, and rapidly cooling to room temperature for later use;
(3) adding 1.5g of sodium dodecyl benzene sulfonate white powder into 17.1g of distilled water, and stirring by a glass rod until the sodium dodecyl benzene sulfonate white powder is completely dissolved to obtain a sodium dodecyl benzene sulfonate aqueous solution as an emulsifier;
(4) adding sodium dodecyl benzene sulfonate aqueous solution and 0.4g of photoinitiator into 10g of water-based acrylic resin, adding a magnetic stirrer, and stirring and emulsifying in a water bath at 60 ℃ for 30min under the condition of 1200r/min of rotation speed to obtain stable core material emulsion;
(5) slowly dripping the wall material modified urea formaldehyde prepolymer into the core material at the rotating speed of 300r/min, gradually adding citric acid crystals, stirring until the citric acid crystals are completely dissolved, testing the pH value of the solution by using a pH test paper, adjusting the pH value to 2.5-3.0, and slowly heating to 70 ℃ for reaction for 3 hours. And carrying out suction filtration on the obtained product, adding distilled water to wash away redundant emulsifier, and finally putting the product into a drying box to be heated and dried for 4 hours at the temperature of 80 ℃, so that the obtained powder is the required microcapsule.
Example 2
(1) Adding 15g of urea and 30g of formaldehyde into a beaker, fully stirring until the urea is dissolved, and adjusting the pH value of the beaker to about 9.0 by using 20g of diethanolamine;
(2) adding 5g of fluororesin and 3g of epoxy resin, fully stirring, adding a magnetic stirrer, stirring for 1h in a constant-temperature water bath at 70 ℃ to obtain slightly viscous transparent modified urea formaldehyde prepolymer solution, and rapidly cooling to room temperature for later use;
(3) adding 2g of sodium dodecyl benzene sulfonate white powder into 13g of distilled water, and stirring by a glass rod until the sodium dodecyl benzene sulfonate white powder is completely dissolved to obtain a sodium dodecyl benzene sulfonate aqueous solution serving as an emulsifier;
(4) adding sodium dodecyl benzene sulfonate aqueous solution and 1g of photoinitiator into 11g of water-based acrylic resin, adding a magnetic stirrer, and stirring and emulsifying in water bath at 60 ℃ for 30min at the rotating speed of 1200r/min to obtain stable core material emulsion;
(5) slowly dripping the wall material modified urea formaldehyde prepolymer into the core material at the rotating speed of 300r/min, gradually adding citric acid crystals, stirring until the citric acid crystals are completely dissolved, testing the pH value of the solution by using a pH test paper, adjusting the pH value to 2.5-3.0, and slowly heating to 70 ℃ for reaction for 3 hours. And carrying out suction filtration on the obtained product, adding distilled water to wash away redundant emulsifier, and finally putting the product into a drying box to be heated and dried for 4 hours at the temperature of 80 ℃, so that the obtained powder is the required microcapsule.
Example 3
(1) Adding 18g of urea and 35g of formaldehyde into a beaker, fully stirring until the urea is dissolved, and adjusting the pH value of the beaker to about 9.0 by using 15g of diethanolamine;
(2) adding 2g of fluororesin and 7.5g of epoxy resin, fully stirring, adding a magnetic stirrer, stirring for 1h in a constant-temperature water bath at 70 ℃ to obtain slightly viscous transparent modified urea formaldehyde prepolymer solution, and rapidly cooling to room temperature for later use;
(3) adding 0.5g of sodium dodecyl benzene sulfonate white powder into 10g of distilled water, and stirring by a glass rod until the sodium dodecyl benzene sulfonate white powder is completely dissolved to obtain a sodium dodecyl benzene sulfonate aqueous solution as an emulsifier;
(4) adding sodium dodecyl benzene sulfonate aqueous solution and 2g of photoinitiator into 10g of water-based acrylic resin, adding a magnetic stirrer, and stirring and emulsifying in water bath at 60 ℃ for 30min at the rotating speed of 1200r/min to obtain stable core material emulsion;
(5) slowly dripping the wall material modified urea formaldehyde prepolymer into the core material at the rotating speed of 300r/min, gradually adding citric acid crystals, stirring until the citric acid crystals are completely dissolved, testing the pH value of the solution by using a pH test paper, adjusting the pH value to 2.5-3.0, and slowly heating to 70 ℃ for reaction for 3 hours. And carrying out suction filtration on the obtained product, adding distilled water to wash away redundant emulsifier, and finally putting the product into a drying box to be heated and dried for 4 hours at the temperature of 80 ℃, so that the obtained powder is the required microcapsule.
Example 4
(1) Adding 30g of urea and 35g of formaldehyde into a beaker, fully stirring until the urea is dissolved, and adjusting the pH value of the beaker to be about 9.0 by using 12.6g of diethanolamine;
(2) adding 1g of fluororesin and 3g of epoxy resin, fully stirring, adding a magnetic stirrer, stirring for 1h in a constant-temperature water bath at 70 ℃ to obtain slightly viscous transparent modified urea formaldehyde prepolymer solution, and rapidly cooling to room temperature for later use;
(3) adding 1g of sodium dodecyl benzene sulfonate white powder into 10g of distilled water, and stirring by a glass rod until the sodium dodecyl benzene sulfonate white powder is completely dissolved to obtain a sodium dodecyl benzene sulfonate aqueous solution serving as an emulsifier;
(4) adding sodium dodecyl benzene sulfonate aqueous solution and 0.4g of photoinitiator into 7g of water-based acrylic resin, adding a magnetic stirrer, and stirring and emulsifying in a water bath at 60 ℃ for 30min under the condition of 1200r/min of rotation speed to obtain stable core material emulsion;
(5) slowly dripping the wall material modified urea formaldehyde prepolymer into the core material at the rotating speed of 300r/min, gradually adding citric acid crystals, stirring until the citric acid crystals are completely dissolved, testing the pH value of the solution by using a pH test paper, adjusting the pH value to 2.5-3.0, and slowly heating to 70 ℃ for reaction for 3 hours. And carrying out suction filtration on the obtained product, adding distilled water to wash away redundant emulsifier, and finally putting the product into a drying box to be heated and dried for 4 hours at the temperature of 80 ℃, so that the obtained powder is the required microcapsule.
Example 5
(1) Adding 20g of urea and 50g of formaldehyde into a beaker, fully stirring until the urea is dissolved, and adjusting the pH value to about 9.0 by using 10g of diethanolamine;
(2) adding 3g of fluororesin and 3.895g of epoxy resin, fully stirring, adding a magnetic stirrer, stirring for 1h in a constant-temperature water bath at 70 ℃ to obtain slightly viscous transparent modified urea formaldehyde prepolymer solution, and rapidly cooling to room temperature for later use;
(3) adding 0.005g of sodium dodecyl benzene sulfonate white powder into 5g of distilled water, and stirring by a glass rod until the sodium dodecyl benzene sulfonate white powder is completely dissolved to obtain a sodium dodecyl benzene sulfonate aqueous solution as an emulsifier;
(4) adding sodium dodecyl benzene sulfonate aqueous solution and 0.1g of photoinitiator into 8g of water-based acrylic resin, adding a magnetic stirrer, and stirring and emulsifying in a water bath at 60 ℃ for 30min under the condition of 1200r/min of rotation speed to obtain stable core material emulsion;
(5) slowly dripping the wall material modified urea formaldehyde prepolymer into the core material at the rotating speed of 300r/min, gradually adding citric acid crystals, stirring until the citric acid crystals are completely dissolved, testing the pH value of the solution by using a pH test paper, adjusting the pH value to 2.5-3.0, and slowly heating to 70 ℃ for reaction for 3 hours. And carrying out suction filtration on the obtained product, adding distilled water to wash away redundant emulsifier, and finally putting the product into a drying box to be heated and dried for 4 hours at the temperature of 80 ℃, so that the obtained powder is the required microcapsule.
Example 6
(1) Adding 20g of urea and 30g of formaldehyde into a beaker, fully stirring until the urea is dissolved, and adjusting the pH value of the beaker to about 9.0 by using 15g of diethanolamine;
(2) adding 3g of fluororesin and 6g of epoxy resin, fully stirring, adding a magnetic stirrer, stirring for 1h in a constant-temperature water bath at 70 ℃ to obtain slightly viscous transparent modified urea formaldehyde prepolymer solution, and rapidly cooling to room temperature for later use;
(3) adding 1.2g of sodium dodecyl benzene sulfonate white powder into 12.4g of distilled water, and stirring by a glass rod until the sodium dodecyl benzene sulfonate white powder is completely dissolved to obtain a sodium dodecyl benzene sulfonate aqueous solution as an emulsifier;
(4) adding a sodium dodecyl benzene sulfonate aqueous solution and 0.4g of a photoinitiator into 12g of water-based acrylic resin, adding a magnetic stirrer, and stirring and emulsifying in a water bath at 60 ℃ for 30min at the rotating speed of 1200r/min to obtain a stable core material emulsion;
(5) slowly dripping the wall material modified urea formaldehyde prepolymer into the core material at the rotating speed of 300r/min, gradually adding citric acid crystals, stirring until the citric acid crystals are completely dissolved, testing the pH value of the solution by using a pH test paper, adjusting the pH value to 2.5-3.0, and slowly heating to 70 ℃ for reaction for 3 hours. And carrying out suction filtration on the obtained product, adding distilled water to wash away redundant emulsifier, and finally putting the product into a drying box to be heated and dried for 4 hours at the temperature of 80 ℃, so that the obtained powder is the required microcapsule.
Example 7
(1) Adding 15g of urea and 30g of formaldehyde into a beaker, fully stirring until the urea is dissolved, and adjusting the pH value of the beaker to be about 9.0 by using 12.1g of diethanolamine;
(2) adding 4g of fluororesin and 8g of epoxy resin, fully stirring, adding a magnetic stirrer, stirring for 1h in a constant-temperature water bath at 70 ℃ to obtain slightly viscous transparent modified urea formaldehyde prepolymer solution, and rapidly cooling to room temperature for later use;
(3) adding 0.4g of sodium dodecyl benzene sulfonate white powder into 20g of distilled water, and stirring by a glass rod until the sodium dodecyl benzene sulfonate white powder is completely dissolved to obtain a sodium dodecyl benzene sulfonate aqueous solution as an emulsifier;
(4) adding sodium dodecyl benzene sulfonate aqueous solution and 1.5g of photoinitiator into 9g of water-based acrylic resin, adding a magnetic stirrer, and stirring and emulsifying in a water bath at 60 ℃ for 30min under the condition of 1200r/min of rotation speed to obtain stable core material emulsion;
(5) slowly dripping the wall material modified urea formaldehyde prepolymer into the core material at the rotating speed of 300r/min, gradually adding citric acid crystals, stirring until the citric acid crystals are completely dissolved, testing the pH value of the solution by using a pH test paper, adjusting the pH value to 2.5-3.0, and slowly heating to 70 ℃ for reaction for 3 hours. And carrying out suction filtration on the obtained product, adding distilled water to wash away redundant emulsifier, and finally putting the product into a drying box to be heated and dried for 4 hours at the temperature of 80 ℃, so that the obtained powder is the required microcapsule.
Performance testing
The microcapsules of examples 1 to 7 were added to a commercially available ordinary wood surface water-based paint in an amount of 5 wt%, and then tested for gloss, wear resistance of a coating film (GB/T3324-2008), impact resistance, and coating repair efficiency, and compared with the commercially available ordinary wood surface water-based paint before the microcapsules were added, the test results are shown in the following table:
Claims (4)
1. the self-repairing microcapsule of the water-based paint on the surface of the wood material is characterized by comprising the following raw materials in parts by weight:
15-30 parts of urea, 30-50 parts of formaldehyde, 10-20 parts of diethanolamine, 1-5 parts of fluororesin, 3-8 parts of epoxy resin, 7-16 parts of water-based acrylic resin, 0.1-2 parts of photoinitiator, 0.005-2 parts of sodium dodecyl benzene sulfonate and 5-20 parts of distilled water; the photoinitiator is benzoin methyl ether;
the preparation method of the wood material surface water-based paint self-repairing microcapsule comprises the following steps:
(1) adding urea into formaldehyde, fully stirring until the urea is dissolved, and adjusting the pH value to 9.0 by using diethanolamine;
(2) adding fluororesin and epoxy resin, fully stirring, adding a magnetic stirrer, uniformly stirring in a constant-temperature water bath at 70 ℃ to obtain a modified urea formaldehyde prepolymer solution, and rapidly cooling to room temperature for later use;
(3) adding sodium dodecyl benzene sulfonate into distilled water, stirring until the sodium dodecyl benzene sulfonate is completely dissolved to obtain a sodium dodecyl benzene sulfonate aqueous solution serving as an emulsifier;
(4) adding a sodium dodecyl benzene sulfonate aqueous solution and a photoinitiator into the water-based acrylic resin, adding a magnetic stirrer for stirring, and stirring and emulsifying in a water bath at 60 ℃ to obtain a stable core material emulsion;
(5) slowly dripping the modified urea formaldehyde prepolymer solution into the core material emulsion at the rotating speed of 300r/min, gradually adding citric acid crystals to adjust the pH to be 2.5-3.0, slowly heating to 65-75 ℃ to react, and then carrying out suction filtration and drying on the obtained product to obtain powder, namely the wood material surface water-based paint self-repairing microcapsule.
2. The wood material surface water-based paint self-repairing microcapsule according to claim 1, which is characterized by comprising the following raw materials in parts by weight: 18-25 parts of urea, 35-45 parts of formaldehyde, 12-18 parts of diethanolamine, 2-4 parts of fluororesin, 3.5-7 parts of epoxy resin, 8-15 parts of water-based acrylic resin, 0.4-1.5 parts of photoinitiator, 0.3-1.5 parts of sodium dodecyl benzene sulfonate and 7-18 parts of distilled water.
3. The wood material surface water-based paint self-repairing microcapsule according to claim 1, wherein in the step (4), the stirring speed of the magnetic stirrer is 1200r/min, and the emulsifying time is 30 min.
4. The wood material surface water-based paint self-repairing microcapsule as claimed in claim 1, 2 or 3, wherein in the step (5), the drying temperature is 80 ℃ and the drying time is 3-5 h.
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