CN119505652A - A fast-curing powder coating and preparation method thereof - Google Patents
A fast-curing powder coating and preparation method thereof Download PDFInfo
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- CN119505652A CN119505652A CN202411459646.6A CN202411459646A CN119505652A CN 119505652 A CN119505652 A CN 119505652A CN 202411459646 A CN202411459646 A CN 202411459646A CN 119505652 A CN119505652 A CN 119505652A
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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
- C09D167/00—Coating compositions based on polyesters obtained by reactions forming a carboxylic ester link in the main chain; Coating compositions based on derivatives of such polymers
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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
- C09D5/03—Powdery paints
- C09D5/033—Powdery paints characterised by the additives
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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
- C08K3/30—Sulfur-, selenium- or tellurium-containing compounds
- C08K2003/3045—Sulfates
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Abstract
本发明公开了一种快速固化的粉末涂料及其制备方法，属于粉末涂料领域。本发明添加羧酸化聚酯树脂和异氰尿酸三缩水甘油酯发生交联反应形成网络结构。固化促进剂能活化羧基官能团，有效促进羧酸化聚酯树脂中的官能团发生反应，有助于提高粉末涂料的固化速度；添加沉淀硫酸钡能降低粉末体系整体粘度；改性流平剂和润湿促进剂协同作用，有效提高粉末涂料的润湿性，降低粉末涂料在固化的熔融过程中内部的表面张力，提升粉末涂料的流平性能，同时使得羧酸化聚酯树脂更容易浸润颜料，加速挥发性物质从表面溢出，同时在脱气剂的协同作用下加速气泡破裂溢出，明显改进涂膜外观，得到平整的涂膜表面，从而解决快速固化带来的涂膜表面粗糙不平的问题。The invention discloses a fast-curing powder coating and a preparation method thereof, and belongs to the field of powder coating. In the invention, a carboxylated polyester resin and triglycidyl isocyanurate are added to generate a cross-linking reaction to form a network structure. A curing accelerator can activate carboxyl functional groups, effectively promote the reaction of functional groups in the carboxylated polyester resin, and help to increase the curing speed of the powder coating; adding precipitated barium sulfate can reduce the overall viscosity of the powder system; the modified leveling agent and the wetting accelerator act synergistically to effectively improve the wettability of the powder coating, reduce the internal surface tension of the powder coating during the curing melting process, and improve the leveling performance of the powder coating. At the same time, the carboxylated polyester resin is more easily infiltrated with pigments, and volatile substances are accelerated to overflow from the surface. At the same time, the bubble bursting and overflowing are accelerated under the synergistic effect of the degassing agent, and the appearance of the coating film is significantly improved to obtain a smooth coating film surface, thereby solving the problem of rough and uneven coating film surface caused by rapid curing.
Description
Technical Field
The invention relates to the field of powder coating preparation, in particular to a rapidly-cured powder coating and a preparation method thereof.
Background
The powder coating is a solid powder synthetic resin coating composed of solid resin, pigment, filler, auxiliary agent and the like. The powder coating has the advantages of no VOC, high utilization rate, easy operation of coating, good comprehensive performance and the like. The powder coating is mainly prepared by the processes of melt extrusion, crushing, grinding and the like. Along with the stricter environmental protection requirements of national and local policies, the application industry of the powder coating is wider and wider, and the market demand is larger and larger.
At present, most powder coatings are overlong in curing time, so that energy resources are consumed too much, and production efficiency is reduced. In the prior art, more rapid curing coatings exist, for example, the invention patent with the Chinese patent application number of CN201710971232.5 discloses a method for realizing rapid curing of powder coatings by utilizing the photo-thermal effect, the photo-thermal conversion filler and resin are uniformly mixed and crushed, then the crushed powder coatings are uniformly arranged on a substrate, but the coating can not give consideration to the performance of a coating film in the forming process, for example, the invention patent with the Chinese patent number of CN201610993976.2 discloses a high-speed infrared curing leveling powder coating and a preparation method thereof, and the components of the powder coating comprise polyester resin, curing agent, leveling agent, benzoin, inorganic filler, wax powder and pigment, but under the condition of quicker film forming, the problem that the surface performance of the coating film is difficult to ensure is existed. Accordingly, the above-mentioned problems to be solved still remain in the prior art.
Disclosure of Invention
Based on the problems of long curing time, low efficiency and poor apparent quality of the powder coating in the prior art, the invention provides a rapidly cured powder coating and a preparation method thereof, and the specific technical scheme is as follows:
The fast-curing powder coating comprises, by mass, 50.0% -60.0% of carboxylated polyester resin, 4.2% -5.0% of triglycidyl isocyanurate, 0.2% -0.3% of a curing accelerator, 0.5% -0.9% of a modified leveling agent, 0.5% -0.9% of a wetting accelerator, 0.1% -0.3% of a degasifying agent, 0.1% -0.5% of a silane coupling agent, 0.1% -0.3% of a toughening agent, 0.1% -0.5% of an antioxidant, 0.2% -0.5% of a hardening wear-resisting agent, 10.0% -30.0% of precipitated barium sulfate and 0% -5.0% of a pigment.
Further, the acid value of the carboxylated polyester resin is 30 mgKOH/g-37 mgKOH/g, the viscosity at 200 ℃ is 3500 mPas-6500 mPas, and the softening point is 103-113 ℃.
Further, the curing accelerator is an onium salt compound.
Further, the wetting accelerator is a methacrylate copolymer.
Further, the degassing agent is a fine amide polymer.
Further, the antioxidant is pentaerythritol ester.
Further, the whiteness of the precipitated barium sulfate is more than 98, and the oil absorption (g/100 g) is 10-20.
In addition, the invention also provides a preparation method of the powder coating, which comprises the following steps of
Adding a modified leveling agent, a silane coupling agent, a wetting accelerator and precipitated barium sulfate into a mixing container, and then introducing high-speed airflow to promote the powder to be in a suspension state under the driving action of the airflow. In the suspension process, powder particles continuously collide with each other and exchange positions, so that materials can be uniformly adhered together, and finally a mixture A is obtained;
The method comprises the steps of adding carboxylated polyester resin, triglycidyl isocyanurate, a curing accelerator, a mixture A modified flatting agent, a wetting accelerator, a degasifying agent, a toughening agent, an antioxidant, a hardening antiwear agent, precipitated barium sulfate and pigment into a three-dimensional rotary water-cooling mixer, and mixing for 20-40min at the rotating speed of 400-500r/min, wherein a central shaft adopts a water-cooling mode, so that the problem that raw materials adhere to walls due to mutual friction and temperature rise of the raw materials in premixing can be effectively solved, and after the raw materials are fully and uniformly mixed in a mixing device, the powder coating capable of being quickly cured is obtained after melt extrusion treatment, tabletting crushing treatment, grinding treatment and sieving treatment.
Further, the melt extrusion treatment process adopts a double-screw extruder, the rotating speed of the double-screw extruder is 120 r/min-150 r/min, the temperature is 100 ℃ to 110 ℃, and the length ratio of a feeding conveying section and a mixing section in the double-screw extruder is 1-2:6-8.
The preparation method of the modified leveling agent comprises the steps of mixing modified polysiloxane and silicon dioxide in a mass ratio of (6-7) (1-4), stirring at a rotating speed of 1000-1200 r/min and a temperature of 45-75 ℃ for 1-2 hours, and drying to obtain the modified leveling agent.
In the scheme, through optimizing the components and the component proportion, the carboxylated polyester resin and triglycidyl isocyanurate undergo a crosslinking reaction to form a network structure. The curing accelerator can effectively promote the reaction of functional groups in carboxylated polyester resin to generate more crosslinking bonds, which is helpful for improving the curing speed of the reaction and greatly shortening the curing time, promotes the modified leveling agent and the wetting accelerator to be adhered on the precipitated barium sulfate under the action of high-speed airflow and the silane coupling agent, so that the modified leveling agent and the wetting accelerator are uniformly dispersed in the melt extrusion process, the effect of reducing the overall viscosity of the powder coating can be achieved by adding the precipitated barium sulfate with low oil absorption, meanwhile, the length of a conveying section and a mixing section of the double-screw extruder is regulated, the components in the powder coating system can be more freely moved and mutually contacted, the components can be more uniformly dispersed, the curing speed can be further accelerated, the leveling property of the powder coating can be promoted by adding the modified leveling agent, the surface tension of the powder coating can be effectively improved, and the powder coating can be melted and leveled in a shorter time. Under the synergistic effect of the wetting accelerator, the wettability of the powder coating is effectively improved, the surface tension in the molten coating is reduced, the carboxylated polyester resin is easier to infiltrate into pigment, and volatile substances such as moisture generated by the crosslinking reaction are accelerated to overflow from the surface. Meanwhile, under the synergistic effect of the degasifying agent, bubbles are accelerated to break and overflow, the appearance of the coating film is obviously improved, the smooth coating film surface is obtained, and the problem that the powder coating in the prior art is rough and uneven in the coating film surface due to rapid solidification is effectively solved.
Detailed Description
The present invention will be described in further detail with reference to the following examples thereof in order to make the objects, technical solutions and advantages of the present invention more apparent. It should be understood that the detailed description and specific examples are intended for purposes of illustration only and are not intended to limit the scope of the invention.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used herein in the description of the invention is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. The term "and/or" as used herein includes any and all combinations of one or more of the associated listed items.
The quick-curing powder coating comprises, by mass, 50.0% -60.0% of carboxylated polyester resin, 4.2% -5.0% of triglycidyl isocyanurate, 0.2% -0.3% of a curing accelerator, 0.5% -0.9% of a modified leveling agent, 0.5% -0.9% of a wetting accelerator, 0.1% -0.3% of a degassing agent, 0.1% -0.5% of a silane coupling agent, 0.1% -0.3% of a toughening agent, 0.1% -0.5% of an antioxidant, 0.2% -0.5% of a hardening wear-resistant agent, 10.0% -30.0% of precipitated barium sulfate and 0% -5.0% of a pigment.
In one embodiment, the carboxylated polyester resin has an acid value of 30mgKOH/g to 37mgKOH/g, a viscosity of 3500 mPas to 6500 mPas at 200 ℃, and a softening point of 103 to 113 ℃.
In one embodiment, the melting range of the triglycidyl isocyanurate is 95-115 ℃, and the epoxy equivalent (g/eq) is less than or equal to 105.
In one embodiment, the cure accelerator is an onium salt compound.
In one embodiment, the wetting enhancer is a methacrylate copolymer.
In one embodiment, the degassing agent is a microfine amide polymer.
In one embodiment, the antioxidant is pentaerythritol ester.
In one embodiment, the pentaerythritol ester has a melting point of 112 ℃ to 129 ℃.
In one embodiment, the stiffening and antiwear agent is polytetrafluoroethylene modified PE wax.
In one embodiment, the median particle size of the polytetrafluoroethylene modified PE wax is 3-6 μm.
In one embodiment, the precipitated barium sulfate has a density of > 98% and an oil absorption (g/100 g) of 10-20.
In addition, the invention also provides a preparation method of the powder coating, which comprises the following steps:
Adding a modified leveling agent, a silane coupling agent, a wetting accelerator and precipitated barium sulfate into a mixing container, and then introducing high-speed airflow to promote the powder to be in a suspension state under the driving action of the airflow. In the suspension process, powder particles continuously collide with each other and exchange positions, so that materials can be uniformly adhered together, and finally a mixture A is obtained;
The carboxylated polyester resin, triglycidyl isocyanurate, a curing accelerator, a mixture A degasser, a toughening agent, an antioxidant, a hardening antiwear agent and pigment are added into a three-dimensional rotary water-cooling mixer and mixed for 20-40min at a rotating speed of 400-500r/min, wherein a central shaft adopts a water-cooling mode, the problem that raw materials are sticky due to mutual friction and temperature rise in premixing can be effectively solved, and after the raw materials are fully and uniformly mixed, the powder coating capable of being quickly cured is obtained after melt extrusion treatment, tabletting crushing treatment, grinding treatment and sieving treatment.
In one embodiment, the melt extrusion treatment process adopts a double-screw extruder for extrusion, the rotating speed of the double-screw extruder is 120-150 r/min, the temperature is 100-110 ℃, and the ratio of the length of a conveying section to the length of a mixing section in the double-screw extruder is 1-2:6-8.
In one embodiment, the preparation method of the modified leveling agent comprises the steps of mixing modified polysiloxane and silicon dioxide in a mass ratio of (6-7) (1-4), stirring at a rotating speed of 1000-1200 r/min and a temperature of 45-75 ℃ for 1-2 hours, and drying to obtain the modified leveling agent.
In one embodiment, the modified polysiloxane is one or both of a polyether modified polysiloxane and a polyester modified polysiloxane.
In the scheme, the powder coating with high curing speed, high effect and excellent apparent coating quality can be obtained by optimizing the components and the component proportion.
Embodiments of the present invention will be described in detail below with reference to specific examples.
Examples 1 to 9:
Examples 1 to 9 differ in the raw materials for preparing the powder coating, specifically as shown in table 1;
the preparation method of the fast-curing powder coating of the embodiments 1 to 9 comprises the following steps:
Mixing polyether modified polysiloxane with the mass ratio of 7:3 and silicon dioxide, stirring for 2 hours at the rotation speed of 1000r/min and the temperature of 65 ℃, and drying to obtain a modified leveling agent;
Adding a modified leveling agent, a silane coupling agent, a wetting accelerator and precipitated barium sulfate into a mixing container, and then introducing high-speed airflow to promote the powder to be in a suspension state under the driving action of the airflow. In the suspension process, powder particles continuously collide with each other and exchange positions, so that materials can be uniformly adhered together, and finally a mixture A is obtained;
The carboxylated polyester resin, triglycidyl isocyanurate, a curing accelerator, a mixture A degasser, a toughening agent, an antioxidant, a hardening antiwear agent and pigment are added into a three-dimensional rotary water-cooling mixer and mixed for 35min at the rotating speed of 450r/min, wherein a central shaft adopts a water-cooling mode, and the problem that raw materials are sticky due to mutual friction and temperature rise of the raw materials in premixing can be effectively solved. After the raw materials are fully and uniformly mixed, carrying out melt extrusion treatment, wherein equipment adopted by the melt extrusion treatment process is a double-screw extruder, the rotating speed of the double-screw extruder is 150r/min, the temperature is 100 ℃, the ratio of the length of a conveying section to the length of a mixing section in the double-screw extruder is 1:6, and after tabletting crushing treatment, grinding treatment and sieving treatment, the rapidly solidified powder coating is obtained.
Comparative examples 1 to 3:
comparative examples 1 to 3 are different from example 9 in the components and the ratio of the components of the production raw materials, and the specific production raw materials and the ratio of the raw materials are shown in Table 1, except that they are the same as in example 9.
Comparative example 4:
Comparative example 4 differs from example 9 in that no modified leveling agent was added in comparative example 4, and the other is the same as in example 9.
Comparative example 5:
comparative example 5 is different from example 9 in that a conventional leveling agent (acrylate leveling agent) was added in comparative example 5, and otherwise the same as in example 9.
TABLE 1 preparation of the starting materials (%)
And carrying out performance test on the powder coating samples prepared in examples 1-9 and the powder coating comparative samples prepared in comparative examples 1-5.
Test example 1 roughness of the coated film was tested with reference to standard GB/T6062-2009 product geometry specification (GPS) surface structure profilometry contact (stylus) instrument nominal properties, the results are shown in table 2.
TABLE 2 roughness
| Group of | Roughness/. Mu.m |
| Example 1 | 0.8 |
| Example 2 | 0.7 |
| Example 3 | 0.7 |
| Example 4 | 0.6 |
| Example 5 | 0.9 |
| Example 6 | 0.7 |
| Example 7 | 0.7 |
| Example 8 | 0.8 |
| Example 9 | 0.8 |
| Comparative example 1 | 2.1 |
| Comparative example 2 | 2.9 |
| Comparative example 3 | 2.4 |
| Comparative example 4 | 3.4 |
| Comparative example 5 | 1.4 |
From the data analysis of Table 2, it is clear that the present application can obtain a coating film with a smooth appearance by optimizing the raw materials and the mixture ratio, which is beneficial to the application.
Test example 2 reference standard GB/T5237.4-2017 aluminium alloy construction section 4 part powder spray section. The results are shown in Table 3.
TABLE 3 test results
From the data analysis of Table 3, the application has excellent bending resistance and stability and obvious overall comprehensive performance of the coating film after optimizing the preparation raw materials and the raw material proportion.
Test example 3 curing by heating, the curing time was recorded and the results are shown in table 4 below.
TABLE 4 curing time
| Group of | Curing temperature/°c | Curing time/min |
| Example 1 | 180 | 4 |
| Example 2 | 180 | 6 |
| Example 3 | 180 | 5 |
| Example 4 | 180 | 4 |
| Example 5 | 180 | 6 |
| Example 6 | 180 | 4 |
| Example 7 | 180 | 4 |
| Example 8 | 180 | 6 |
| Example 9 | 180 | 5 |
| Comparative example 1 | 180 | 10 |
| Comparative example 2 | 180 | 9 |
| Comparative example 3 | 180 | 10 |
| Comparative example 4 | 180 | 11 |
| Comparative example 5 | 180 | 9 |
As can be seen from the data analysis of Table 4, the application helps to shorten the curing time of the powder coating by optimizing the preparation raw materials and the mixture ratio, ensures the comprehensive performance of the coating film, can achieve the balance of the curing degree and the curing time, and helps to improve the production efficiency.
The technical features of the above-described embodiments may be arbitrarily combined, and all possible combinations of the technical features in the above-described embodiments are not described for brevity of description, however, as long as there is no contradiction between the combinations of the technical features, they should be considered as the scope of the description.
The above examples illustrate only a few embodiments of the invention, which are described in detail and are not to be construed as limiting the scope of the invention. It should be noted that it will be apparent to those skilled in the art that several variations and modifications can be made without departing from the spirit of the invention, which are all within the scope of the invention. Accordingly, the scope of protection of the present invention is to be determined by the appended claims.
Claims (10)
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