CN110317520A - A kind of low temperature cured powder coating and preparation method thereof - Google Patents

A kind of low temperature cured powder coating and preparation method thereof Download PDF

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Publication number
CN110317520A
CN110317520A CN201910606931.9A CN201910606931A CN110317520A CN 110317520 A CN110317520 A CN 110317520A CN 201910606931 A CN201910606931 A CN 201910606931A CN 110317520 A CN110317520 A CN 110317520A
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China
Prior art keywords
low temperature
filler
powder coating
cured powder
temperature cured
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CN201910606931.9A
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Chinese (zh)
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苗雪峰
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Anhui Shun Bang Fine Chemical Co Ltd
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Anhui Shun Bang Fine Chemical Co Ltd
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Priority to CN201910606931.9A priority Critical patent/CN110317520A/en
Publication of CN110317520A publication Critical patent/CN110317520A/en
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING 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
    • C09D163/00Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING 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
    • C09D7/00Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40Additives
    • C09D7/60Additives non-macromolecular
    • C09D7/61Additives non-macromolecular inorganic
    • C09D7/62Additives non-macromolecular inorganic modified by treatment with other compounds
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/30Sulfur-, selenium- or tellurium-containing compounds
    • C08K2003/3009Sulfides
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/011Nanostructured additives

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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 discloses a kind of low temperature cured powder coating and preparation method thereof, the raw material including following weight parts: bisphenol A type epoxy resin 80-100, low temperature curing agent 15-20, modified filler 60-80, levelling agent 1.5-2.5, defoaming agent 0.3-0.5, styrax 0.1-0.2.Low temperature cured powder coating of the invention has excellent levelability and adhesive force, can rapid curing at low temperature, form that good mechanical property, adhesive force is high, flawless film on ground.

Description

A kind of low temperature cured powder coating and preparation method thereof
Technical field
The present invention relates to powder coating technology fields more particularly to a kind of low temperature cured powder coating and preparation method thereof.
Background technique
With the continuous improvement that energy conservation and environmental protection requires, the powdery paints advantage energy saving, nuisanceless, high-efficient with it is by people Favor.General powdery paints usually requires at a high temperature of 180-200 DEG C, toasts just by the long-time of 20-30min The defects of energy crosslinking curing film forming, not only consumes energy, is time-consuming, but also coating is easy to appear shrinkage cavity, orange peel, also makes it in timber, modeling Coating on a variety of substrates such as material, electronic component, temperature-sensitive material is restricted.Powdery paints low-temperature setting technology, which becomes, to be worked as A preceding developing focus.
Low temperature cured powder coating mainly makes coating form a film at relatively low temperature, and a solidified mistake Journey.Complete the solidification of coating system at a lower temperature, and keep the good quality of film, is low-temperature setting powder The key of last coating development.On the one hand, when low-temperature setting, since melting of the fusible materials such as resin, curing agent in low temperature is viscous Bigger, mobilization force decline is spent, and the wetability of the components such as filler is declined, is easy to cause the levelability of film to be deteriorated, not yet Abundant levelling begins to solidify, and leads to the defects of tangerine line, pin hole occur, and mechanical degradation;On the other hand, solid with high temperature Change is compared, and film is lower to the low-temperature setting adhesive force of ground, becomes an important restraining factors of powdery paints application.Cause How this, guarantee the good levelability of film, improves the mechanical performance and adhesive force of film, is current low temperature cured powder coating The problem of urgently improving.
Summary of the invention
The purpose of the invention is to make up the defect of prior art, a kind of low temperature cured powder coating and its preparation are provided Method makes low temperature cured powder coating have excellent levelability and adhesive force, can rapid curing at low temperature, the shape on ground At good mechanical property, adhesive force height, flawless film.
The present invention is achieved by the following technical solutions:
A kind of low temperature cured powder coating, the raw material including following weight parts:
Bisphenol A type epoxy resin 80-100, low temperature curing agent 15-20, modified filler 60-80, levelling agent 1.5-2.5 disappear Infusion 0.3-0.5, styrax 0.1-0.2.
The epoxide equivalent of the bisphenol A type epoxy resin is 700-740, and softening point is 86-92 DEG C.
The low temperature curing agent is phenols curing agent.
The modified filler the preparation method is as follows:
(a) coupling agent is grafted filler, methyl acrylate and methanol by weight (20-30): (1-2): 100 mix after it is normal Temperature reaction 12-24h, obtains graft polymerization preformer filler, by weight by the graft polymerization preformer filler, ethylenediamine and methanol after being filtered, washed (20-30): (3-5): normal-temperature reaction 12-24h is obtained in 70-80 DEG C of vacuum drying 4-6h after being filtered, washed after 100 mixing PAMAM is grafted filler;
(b) by ammonium paramolybdate, thiocarbamide and water by weight (1-1.2): (2-2.5): dissolving after 100 mixing and mixed completely Close liquid, then by PAMAM that step (a) obtains grafting filler with the mixed liquor by weight (10-20): 100 mix after divide It dissipates uniformly, pH is adjusted to 5-6, in 140-160 DEG C of hydrothermal synthesis reaction 4-6h in ptfe autoclave, is filtered, washed Afterwards in 70-80 DEG C of dry 4-6h to get modified filler.
Coupling agent grafting filler the preparation method is as follows: by silane resin acceptor kh-550 and filler by weight (1- 2): 100 after evenly mixing in 100-120 DEG C of isothermal holding 20-30min, cooling to obtain coupling agent grafting filler.
The filler is selected from one of kaolin, precipitated silica, mica powder, silica flour or several mixing.
The preparation method of low temperature cured powder coating, the specific steps are as follows: each component is weighed by weight, by double after mixing Screw extruder carry out melting extrusion, through supercooling, crushing, sieving to get.
The application method of low temperature cured powder coating, the specific steps are as follows: low temperature cured powder coating electrostatic spraying exists Substrate surface forms film then in 120-130 DEG C of solidification 15-20min.
Beneficial effects of the present invention are as follows:
The present invention first passes through silane coupling agent and activates to filler surface, is then to connect with methyl acrylate, ethylenediamine Branch reactant will have the macromole polyamide amine (PAMAM) of dendritic structure in filler surface grafting, obtain PAMAM grafting Filler, then using ammonium paramolybdate, thiocarbamide as presoma, pass through hydrothermal synthesis method under suitable conditions for proper amount of nano molybdenum disulfide It is supported on PAMAM grafting filler, obtains modified filler, be added in low temperature cured powder coating system, using PAMAM to filling out The grafting of material improves the dispersibility of coating system and the adhesion of itself and ground, is filled out using the load raising of nano molybdenum disulfide The lubricity of material, and then improve the levelability of coating system.Low temperature cured powder coating formula of the invention can be compared with low temperature Lower rapid curing is spent, while keeping good coat film flatness, mechanical strength and the high adhesion force with ground, is had extremely excellent Good comprehensive performance.
Specific embodiment
Embodiment 1
A kind of low temperature cured powder coating, the raw material including following weight parts:
Bisphenol A type epoxy resin E-1280, phenols curing agent W-115315, modified filler 60, levelling agent BYK-360P 1.5, defoaming agent BYK-066N 0.3, styrax 0.1.
The epoxide equivalent of the bisphenol A type epoxy resin is 700, and softening point is 86 DEG C.
The modified filler the preparation method is as follows:
(a) normal-temperature reaction after mixing coupling agent grafting filler, methyl acrylate by weight 20:1:100 with methanol 12h obtains graft polymerization preformer filler after being filtered, washed, after graft polymerization preformer filler, ethylenediamine are mixed with methanol by weight 20:3:100 Normal-temperature reaction 12h obtains PAMAM grafting filler in 70 DEG C of vacuum drying 4h after being filtered, washed;
(b) it is dissolved after mixing ammonium paramolybdate, thiocarbamide and water by weight 1:2:100 and obtains mixed liquor completely, then will The PAMAM grafting filler that step (a) obtains is uniformly dispersed after mixing with mixed liquor by weight 10:100, pH is adjusted to 5, poly- In 140 DEG C of hydrothermal synthesis reaction 4h in tetrafluoroethene reaction kettle, in 70 DEG C of dry 4h to get modified filler after being filtered, washed.
Coupling agent be grafted filler the preparation method is as follows: by silane resin acceptor kh-550 and silica flour by weight 1:100 It is cooling to obtain coupling agent grafting filler after evenly mixing in 100 DEG C of isothermal holding 20min.
The preparation method of low temperature cured powder coating, the specific steps are as follows: each component is weighed by weight, by double after mixing Screw extruder carry out melting extrusion, through supercooling, crushing, sieving to get.
Embodiment 2
A kind of low temperature cured powder coating, the raw material including following weight parts:
Bisphenol A type epoxy resin E-12100, phenols curing agent W-115320, modified filler 80, levelling agent BYK-360P 2.5, defoaming agent BYK-066N 0.5, styrax 0.2.
The epoxide equivalent of bisphenol A type epoxy resin is 740, and softening point is 92 DEG C.
Modified filler the preparation method is as follows:
(a) normal-temperature reaction after mixing coupling agent grafting filler, methyl acrylate by weight 30:2:100 with methanol For 24 hours, graft polymerization preformer filler is obtained after being filtered, washed, after graft polymerization preformer filler, ethylenediamine are mixed with methanol by weight 30:5:100 Normal-temperature reaction for 24 hours, in 80 DEG C of vacuum drying 6h after being filtered, washed, obtains PAMAM grafting filler;
(b) it is dissolved after mixing ammonium paramolybdate, thiocarbamide and water by weight 1.2:2.5:100 and obtains mixed liquor completely, so It is uniformly dispersed after the PAMAM grafting filler that step (a) obtains is mixed with mixed liquor by weight 20:100 afterwards, pH is adjusted to 6, In 160 DEG C of hydrothermal synthesis reaction 6h in ptfe autoclave, filled out after being filtered, washed in 80 DEG C of dry 6h to get modification Material.
Coupling agent be grafted filler the preparation method is as follows: by silane resin acceptor kh-550 and silica flour by weight 2:100 It is cooling to obtain coupling agent grafting filler after evenly mixing in 120 DEG C of isothermal holding 30min.
The preparation method of low temperature cured powder coating, the specific steps are as follows: each component is weighed by weight, by double after mixing Screw extruder carry out melting extrusion, through supercooling, crushing, sieving to get.
Comparative example 1
This comparative example is the control of embodiment 1, with being distinguished as embodiment 1, replaces being modified using coupling agent grafting filler Filler specifically includes the raw material of following weight parts:
Bisphenol A type epoxy resin E-1280, phenols curing agent W-115315, coupling agent are grafted filler 60, levelling agent BYK- 360P 1.5, defoaming agent BYK-066N 0.3, styrax 0.1.
The epoxide equivalent of bisphenol A type epoxy resin is 700, and softening point is 86 DEG C.
Coupling agent be grafted filler the preparation method is as follows: by silane resin acceptor kh-550 and silica flour by weight 1:100 It is cooling to obtain coupling agent grafting filler after evenly mixing in 100 DEG C of isothermal holding 20min.
Specific step is as follows for preparation method: weighing each component by weight, is melted after mixing by double screw extruder Melt extrusion, through supercooling, crushing, sieving to get.
Comparative example 2
This comparative example is the control of embodiment 1, with being distinguished as embodiment 1, replaces modified filler, tool using conventional fillers Body includes the raw material of following weight parts:
Bisphenol A type epoxy resin E-1280, phenols curing agent W-115315, silica flour 60, levelling agent BYK-360P 1.5, Defoaming agent BYK-066N 0.3, styrax 0.1.
The epoxide equivalent of bisphenol A type epoxy resin is 700, and softening point is 86 DEG C.
Specific step is as follows for preparation method: weighing each component by weight, is melted after mixing by double screw extruder Melt extrusion, through supercooling, crushing, sieving to get.
By powder coating electrostatic spraying made from embodiment 1-2 and comparative example 1-2 in surface of aluminum plate, then in 120 DEG C Solidify 15min, forms film.The film of formation is tested for the property, wherein the test method of appearance is to estimate, adhesive force, Impact strength and flexible test method respectively according to GB/T 9286-1998 " cross cut test of paint and varnish paint film ", GB/T 1732-1993 " paint film impact resistance measuring method " and GB/T 1731-1993 " paint film flexibility measuring method ", test result is such as Shown in following table:
It can be seen that compared with the low temperature cured powder coating of addition conventional fillers and coupling agent modified filler, the present invention Low temperature cured powder coating formula can rapid curing at a lower temperature, while keeping good coat film flatness, machinery Intensity and high adhesion force with ground have superfine comprehensive performance.

Claims (8)

1. a kind of low temperature cured powder coating, which is characterized in that the raw material including following weight parts:
Bisphenol A type epoxy resin 80-100, low temperature curing agent 15-20, modified filler 60-80, levelling agent 1.5-2.5, defoaming agent 0.3-0.5, styrax 0.1-0.2.
2. a kind of low temperature cured powder coating according to claim 1, which is characterized in that the bisphenol A type epoxy resin Epoxide equivalent be 700-740, softening point be 86-92 DEG C.
3. a kind of low temperature cured powder coating according to claim 1, which is characterized in that the low temperature curing agent is phenols Curing agent.
4. a kind of low temperature cured powder coating according to claim 1, which is characterized in that the preparation side of the modified filler Method is as follows:
(a) coupling agent is grafted filler, methyl acrylate and methanol by weight (20-30): (1-2): 100 mix after room temperature it is anti- 12-24h is answered, graft polymerization preformer filler is obtained after being filtered, washed, by the graft polymerization preformer filler, ethylenediamine and methanol by weight (20- 30): (3-5): normal-temperature reaction 12-24h obtains PAMAM in 70-80 DEG C of vacuum drying 4-6h after being filtered, washed after 100 mixing It is grafted filler;
(b) by ammonium paramolybdate, thiocarbamide and water by weight (1-1.2): (2-2.5): dissolving after 100 mixing and mixed completely Liquid, then by weight (10-20) by PAMAM that step (a) obtains grafting filler and the mixed liquor: 100 mix after disperse Uniformly, pH is adjusted to 5-6, in 140-160 DEG C of hydrothermal synthesis reaction 4-6h in ptfe autoclave, after being filtered, washed In 70-80 DEG C of dry 4-6h to get modified filler.
5. a kind of low temperature cured powder coating according to claim 4, which is characterized in that the coupling agent grafting filler The preparation method is as follows: by silane resin acceptor kh-550 and filler by weight (1-2): 100 protect in 100-120 DEG C after evenly mixing Temperature processing 20-30min, the cooling coupling agent that obtains are grafted filler.
6. a kind of low temperature cured powder coating according to claim 5, which is characterized in that the filler be selected from kaolin, One of precipitated silica, mica powder, silica flour or several mixing.
7. the preparation method of low temperature cured powder coating described in claim 1, which is characterized in that specific step is as follows: by weight Amount weigh each component, after mixing by double screw extruder progress melting extrusion, through supercooling, crushing, sieving to get.
8. a kind of application method of low temperature cured powder coating described in claim 1-7, which is characterized in that specific steps are such as Under: by low temperature cured powder coating electrostatic spraying in substrate surface, then in 120-130 DEG C of solidification 15-20min, form film.
CN201910606931.9A 2019-07-06 2019-07-06 A kind of low temperature cured powder coating and preparation method thereof Pending CN110317520A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112920684A (en) * 2021-02-26 2021-06-08 北京碧海云智新材料技术有限公司 Low-temperature curing powder coating and preparation method and application thereof
CN113249015A (en) * 2021-05-08 2021-08-13 江门市皇宙实业有限公司 High-temperature-resistant powder coating and preparation method thereof
CN113321992A (en) * 2021-05-13 2021-08-31 江门市皇宙实业有限公司 Antibacterial powder coating
CN115044173A (en) * 2022-07-11 2022-09-13 中山超分子新材料有限公司 Corrosion-resistant high-elasticity composite fiber and preparation method thereof

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112920684A (en) * 2021-02-26 2021-06-08 北京碧海云智新材料技术有限公司 Low-temperature curing powder coating and preparation method and application thereof
CN113249015A (en) * 2021-05-08 2021-08-13 江门市皇宙实业有限公司 High-temperature-resistant powder coating and preparation method thereof
CN113321992A (en) * 2021-05-13 2021-08-31 江门市皇宙实业有限公司 Antibacterial powder coating
CN115044173A (en) * 2022-07-11 2022-09-13 中山超分子新材料有限公司 Corrosion-resistant high-elasticity composite fiber and preparation method thereof

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