CN110343445A - A kind of powder paint compositions and its preparation method and application - Google Patents
A kind of powder paint compositions and its preparation method and application Download PDFInfo
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- CN110343445A CN110343445A CN201910647235.2A CN201910647235A CN110343445A CN 110343445 A CN110343445 A CN 110343445A CN 201910647235 A CN201910647235 A CN 201910647235A CN 110343445 A CN110343445 A CN 110343445A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- 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
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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
- 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
- C09D5/16—Antifouling paints; Underwater paints
- C09D5/1656—Antifouling paints; Underwater paints characterised by the film-forming substance
- C09D5/1662—Synthetic film-forming substance
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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
- C09D5/16—Antifouling paints; Underwater paints
- C09D5/1687—Use of special 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
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- 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
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- 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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- 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
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2312/00—Crosslinking
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Abstract
The present invention provides a kind of powder paint compositions and its preparation method and application, and the raw material for preparing of the powder paint compositions includes following ingredient: 51~90 parts by weight of epoxy resin, 40~60 parts by weight of terminal carboxyl polyester resin, 0.1~10 parts by weight of 0.5~10 parts by weight of highly-branched polymers, 0.2~5 parts by weight of low surface energy auxiliary agent and Isocyanates curing agent.The powder paint compositions by each component by dispersing, mixing, squeeze out, and then the method for tabletting and crushing is prepared.Powder paint compositions provided by the invention are realized low-temperature fast-curing, it is highly applicable to the coating of the surfaces of heat-sensitive substrates such as timber, glass, paper and plastics, the hardness of paint film is high after solidification, flexibility is good, crosslink density is high, has excellent anti-graffiti property and anti-stain characteristic.
Description
Technical field
The invention belongs to technical field of polymer materials, and in particular to a kind of powder paint compositions and preparation method thereof and
Using.
Background technique
The solid powdery synthesis tree that powdery paints is made of resin, curing agent, inorganic filler, pigment and auxiliary agent etc.
Grease coating material is different with usual vehicle type coating and water paint, the decentralized medium of powdery paints not instead of organic solvent or water,
Air.Powdery paints can 100% film forming, it is a kind of coating of real environmental protection that solvent-free pollution, which will not cause water pollution,
And have the characteristics that low energy consumption, recyclable, it is widely used in construction material, household electrical appliances furniture, engineering machinery, electric and work
The fields such as industry anti-corrosion.With the continuous development of powdery paints, people to the performance of film there has also been new requirement, not only want by coating
In terms of realize to the safeguard function of substrate more to meet the needs of to its external appreciation effect, especially build
It builds, in communal facility and household electrical appliances field of furniture, there is dirt-resistant, anti-graffiti performance after coating film forming, on the one hand can make
Substrate itself keeps beautiful, on the other hand can reduce cleaning difficulty, save cleaning cost.Therefore, development has dirt-resistant, prevents
The powdery paints of scribble performance has great importance.
CN103194140B discloses a kind of extra-weather-proof powdery paints of automatically cleaning and preparation method thereof, in the powdery paints
The terminal carboxyl polyester granular system and fluorocarbon resin granular system for being 4:1~1:4 including weight fraction ratio, terminal carboxyl polyester particle
It respectively include corresponding matrix resin, curing agent, auxiliary agent and pigments and fillers, and fluorocarbon resin in system and fluorocarbon resin granular system
Granular system also contains TiO2Nanoparticle assigns the good inoxidizability of coating.The powdery paints can be solid at 200 DEG C
Change, adhesive force is good, resistance to ag(e)ing and stability are high for the painting film base material of formation, and fluorocarbon resin system makes film with excellent
Weatherability and self-cleaning performance.
CN101712834A discloses a kind of doodling prevention powder coating and preparation method thereof, includes in the powdery paints
150~250 parts of acrylic resins, 30~40 parts of propylene acid as curing agent, 20~100 parts of titanium dioxides and 1~20 part of auxiliary agent, wherein third
Olefin(e) acid resin is glycidyl acrylic resin, and propylene acid as curing agent is representative examples of saturated aliphatic diacid；The powdery paints has
Formula is simple, coated solidified is convenient, chemical resistance is excellent, the features such as can quickly wiping, and is suitable for blank, communal facility etc.
Coating.
CN104231906A discloses a kind of doodling prevention powder coating, the powdery paints include matrix resin, curing agent,
Pigments and fillers and auxiliary agent, wherein matrix resin is the composition of low hydroxy polyester resin and high hydroxy polyester resin, and curing agent is envelope
Closed form carbimide；The powdery paints production cost is low, has many advantages, such as high-leveling, high surface hardness and anti-pollution.
CN109354996A discloses a kind of powdery paints and application thereof, and the component of the powdery paints includes polyurethane tree
Rouge, cyanate, nanometer spar barium and BYK defoaming micronization wax；Wherein the weight average molecular weight of polyurethane resin is 3000~6000；
The powdery paints solidifies at 200 DEG C, and the paint film of formation has resistance to scribble, easy to clean, scratch resistance, and can keep coating for a long time
Surface effect.
However in the prior art, have the powdery paints of dirt-resistant, antigraffiti properties mostly with polyurethane, polyester or third
Olefin(e) acid is matrix resin, needs the film-forming under 200 DEG C of high-temperature bakings, and this harsh condition of cure significantly limits base
The range of choice of material.The fields such as interior decoration, furniture are expanded to powdery paints application field, using timber, plastics as generation
The high temperature curing conditions of the unbearable powdery paints in the prior art of the heatsensitive substrates of table, it is even more impossible to realize the mechanicalness of paint film
Energy and surface property.
Based on this, a kind of low-temperature curable powder suitable for heatsensitive substrates with anti-graffiti anti-stain characteristic energy is developed
Last coating is the research emphasis of this field.
Summary of the invention
In view of the deficiencies of the prior art, the purpose of the present invention is to provide a kind of powder paint compositions and preparation method thereof
And application, the powder paint compositions use epoxy resin for matrix resin, arrange in pairs or groups terminal carboxyl polyester resin and curing agent reality
The low-temperature fast-curing and high crosslink density of existing film, and pass through the coordinated of highly-branched polymers and low surface energy auxiliary agent
Make film that there is dirt-resistant, antigraffiti properties.
To achieve this purpose, the present invention adopts the following technical scheme:
In a first aspect, the present invention provides a kind of powder paint compositions, the powder paint compositions prepare raw material packet
Include following ingredient:
It is on the one hand because of asphalt mixtures modified by epoxy resin using epoxy resin as matrix resin in powder paint compositions provided by the invention
Epoxy group and pendant hydroxyl group in rouge molecule all have reactivity, can react solidification with a variety of crosslinking agents, and solidification temperature is low,
Under the conditions of 140~160 DEG C can completion of cure, therefore be highly applicable in the thermal sensitivity such as timber, paper, glass, RPVC, POM
Coating on substrate；Another aspect epoxy resin can be formed by curing with functional resin or auxiliary agent by chemistry key connection
Film has both mechanical performance, patience and appearance.Carboxyl in the present invention in terminal carboxyl polyester resin molecule on the one hand can
With with the pendant hydroxyl group esterification and crosslinking in epoxy resin, on the other hand can promote that epoxy ring-opening, that further crosslinking occurs is anti-
It answers；More importantly facilitating the hardness and punching that promote paint film containing the rigid chain based on phenyl ring in terminal carboxyl polyester resin
Hitting property, and richness and glossiness are good after polyester resin film forming, effectively compensate for the deficiency of epoxy resin paint film in appearance.
- NCO the functional group of Isocyanates curing agent can be with epoxy resin, terminal carboxyl polyester resin, highly branched poly- in the present invention
- OH the reaction in object and low surface energy auxiliary agent is closed, form compact and stable cross-linked network is formed.
Film with dirt-resistant, antigraffiti properties in order to obtain in the present invention, creatively by low surface energy auxiliary agent and
Highly-branched polymers combine, and wherein the special tufted structure of highly-branched polymers can promote powder paint compositions to exist
Mobility under molten condition facilitates the film coated surface for obtaining good leveling property；And hyperbranched point of highly-branched polymers
Minor structure can be combined between low surface energy auxiliary agent, there is low surface energy auxiliary agent under the drive of highly-branched polymers
Effect floats up to film coated surface, to reduce the surface energy of film, realizes dirt-resistant, the antigraffiti properties of film；In addition, height is propped up
Fluidized polymer drives low surface energy auxiliary agent to rise to film coated surface, and avoid low surface energy auxiliary agent from being cured causes in coat inside
The reduction of its effective concentration reduces the usage amount of low surface energy auxiliary agent and reducing its loss.The highly-branched polymers
Dosage should control in the framework of the present definition, if its additive amount is too low, low surface energy auxiliary agent can not be effectively facilitated
It floats, is unable to get low-surface-energy film；If its adding too much can destroy the continuity of film, the machinery of film is influenced
Performance.
In the present invention, the dosage of the epoxy resin can for 52 parts by weight, 54 parts by weight, 56 parts by weight, 58 parts by weight,
60 parts by weight, 63 parts by weight, 65 parts by weight, 67 parts by weight, 70 parts by weight, 72 parts by weight, 75 parts by weight, 78 parts by weight, 80 weights
Specific point value between amount part, 82 parts by weight, 85 parts by weight, 87 parts by weight or 89 parts by weight and above-mentioned point value, as space is limited
And for concise consideration, specific point value that range described in the present invention no longer exclusive list includes.
The dosage of the terminal carboxyl polyester resin can be 42 parts by weight, 44 parts by weight, 46 parts by weight, 48 parts by weight, 50
Specific point value between parts by weight, 53 parts by weight, 55 parts by weight, 57 parts by weight or 59 parts by weight and above-mentioned point value, is limited to a piece
Width and for concise consideration, the specific point value that range described in the present invention no longer exclusive list includes.
The dosage of the highly-branched polymers can be 0.6 parts by weight, 0.8 parts by weight, 1 parts by weight, 3 parts by weight, 5 weights
Specific point value between amount part, 7 parts by weight or 9 parts by weight and above-mentioned point value, as space is limited and for concise consideration, originally
The specific point value that range described in invention no longer exclusive list includes.
The dosage of the low surface energy auxiliary agent can be 0.3 parts by weight, 0.5 parts by weight, 0.7 parts by weight, 1 parts by weight, 1.2
Parts by weight, 1.5 parts by weight, 1.7 parts by weight, 2 parts by weight, 2.3 parts by weight, 2.5 parts by weight, 2.8 parts by weight, 3 parts by weight, 4 weights
The specific point value between part or 4.5 parts by weight and above-mentioned point value is measured, as space is limited and for concise consideration, the present invention is not
The specific point value that range described in exclusive list includes again.
The dosage of the Isocyanates curing agent can be 0.3 parts by weight, 0.5 parts by weight, 0.7 parts by weight, 1 weight
Specific point value between part, 3 parts by weight, 5 parts by weight, 7 parts by weight or 9 parts by weight and above-mentioned point value, as space is limited and for
Concise consideration, the specific point value that range described in the present invention no longer exclusive list includes.
Preferably, the epoxy resin includes following ingredient:
40~60 parts by weight of bisphenol-type epoxy resin
10~20 parts by weight of novolac epoxy resin
1~10 parts by weight of aliphatic epoxy resin.
Preferably, the bisphenol-type epoxy resin is selected from bisphenol A type epoxy resin, bisphenol-s epoxy resin, bisphenol-f type
In epoxy resin, bisphenol-A epoxy resin or tetrabormated bisphenol A type epoxy resin any one or at least two group
It closes.
Preferably, the novolac epoxy resin is linear phenolic epoxy resin.
Epoxy resin in the present invention is the composition of a variety of epoxy resin, and wherein the degree of functionality of novolac epoxy resin is greater than
2, there are more reactivity sites, facilitate the crosslink density for promoting the powder paint compositions；Aliphatic epoxy tree
Rouge is added to introduce the soft segment of alkyl in powdery paints, improves the flexibility of film.Above-mentioned three kinds of epoxy resin
Crosslink density height, the paint film with hardness and flexible sexual balance can be just obtained with the parts by weight of composition that the present invention limits；If exceeding
The framework of the present definition, novolac epoxy resin content is too low, then can not effectively improve crosslink density, novolac epoxy resin content
It is excessively high, then it is firmly crisp to may cause paint film；The too low flexibility that will affect paint film of the content of aliphatic epoxy resin, it is excessively high, cause
Hardness of paint film is inadequate.
Commercial product can be selected in epoxy resin of the present invention, thus not to the molecular weight of epoxy resin and epoxide equivalent into
Row particular determination.Illustratively, the good E12 of Anhui U.S. can be selected in bisphenol-type epoxy resin (such as bisphenol A type epoxy resin)
(604) or the CTAB of Switzerland Ciba-Geigy company can be selected in the CYD-014 of Ba Ling petrochemical industry etc., novolac epoxy resin
The DER732 or DER736 etc. of Tao Shi can be selected in the DER672U etc. of Aradur7255 or Tao Shi, aliphatic epoxy resin.
In the present invention, the dosage of the bisphenol-type epoxy resin can be 42 parts by weight, 44 parts by weight, 46 parts by weight, 48
It is specific between parts by weight, 50 parts by weight, 53 parts by weight, 55 parts by weight, 57 parts by weight or 59 parts by weight and above-mentioned point value
Value, as space is limited and for concise consideration, the specific point value that range described in the present invention no longer exclusive list includes.
The dosage of the novolac epoxy resin can be 11 parts by weight, 12 parts by weight, 13 parts by weight, 14 parts by weight, 15 weights
Specific point value between amount part, 16 parts by weight, 17 parts by weight, 18 parts by weight or 19 parts by weight and above-mentioned point value, as space is limited
And for concise consideration, specific point value that range described in the present invention no longer exclusive list includes.
The dosage of the aliphatic epoxy resin can be 1 parts by weight, 2 parts by weight, 3 parts by weight, 4 parts by weight, 5 weight
Specific point value between part, 6 parts by weight, 7 parts by weight, 8 parts by weight or 9 parts by weight and above-mentioned point value, as space is limited and for
Concise consideration, the specific point value that range described in the present invention no longer exclusive list includes.
Preferably, the terminal carboxyl polyester resin is the mixture of high acid value polyester resin and low acid value polyester resin.
Preferably, the mass ratio of the high acid value polyester resin and low acid value polyester resin is 1:(4~9), such as 1:
4.5,1:5,1:6,1:7,1:8 or 1:8.5 etc..
Preferably, the acid value of the high acid value polyester resin is 70~90mg KOH/g, such as 72mg KOH/g, 74mg
KOH/g、75mg KOH/g、77mg KOH/g、80mg KOH/g、82mg KOH/g、84mg KOH/g、85mg KOH/g、87mg
KOH/g or 89mg KOH/g etc..
Preferably, the acid value of the low acid value polyester resin is 10~40mg KOH/g, such as 12mg KOH/g, 15mg
KOH/g、17mg KOH/g、20mg KOH/g、23mg KOH/g、25mg KOH/g、27mg KOH/g、30mg KOH/g、33mg
KOH/g, 35mg KOH/g, 37mg KOH/g or 39mg KOH/g etc..
On the one hand terminal carboxyl polyester resin of the present invention is used as curing agent, provide and crosslink instead with matrix epoxy resin
The carboxyl answered, on the other hand the rigid chain segments such as phenyl ring in its molecular structure impart powder paint compositions of the present invention at
Glossiness, richness and hardness after film.The terminal carboxyl polyester resin is high acid value polyester resin and low acid value polyester tree
The combination of rouge, wherein a large amount of carboxyls in high acid value polyester resin are crosslinked with the epoxy group in epoxy resin reacts, low acid
It remains more hydroxyl in value polyester resin to react with-the NCO in Isocyanates curing agent, two kinds of cross-linking reactions are sent out simultaneously
It is raw, the fine and close three-dimensional net structure of interpenetrating is formed after so that powder paint compositions of the present invention is formed a film, to assign paint film
High crosslink density, high rigidity and antigraffiti properties.If the mass ratio of the high acid value polyester resin and low acid value polyester resin
Beyond the framework of the present definition, the excessively few crosslink density that then will affect with epoxy resin of high acid value polyester resin, high acid value gathers
Ester resin excessively then will affect the yellowing resistance after powder paint compositions form a film and flexibility.
Preferably, the dosage of the low surface energy auxiliary agent is 0.2~3 parts by weight.
Preferably, the low surface energy auxiliary agent is organosilicon auxiliary agent and/or fluorine auxiliary agent.
Preferably, the organosilicon auxiliary agent is organic-silicon-modified hydroxy acrylate, hydroxy silicon oil or organic-silicon-modified hydroxyl
In base polyester resin any one or at least two combination.
Preferably, the fluorine auxiliary agent is fluorine richness hydroxy acrylate.
Preferably, the highly-branched polymers are dendritic or dissaving polymer, are further preferably surpassed
Branched polymer.
Preferably, the dissaving polymer is superbrnaching end-hydroxy polyester.
Preferably, the number-average molecular weight of the superbrnaching end-hydroxy polyester be 500~3000g/mol, such as 550g/mol,
600g/mol、800g/mol、1000g/mol、1200g/mol、1500g/mol、1800g/mol、2000g/mol、2300g/
Mol, 2500g/mol, 2700g/mol or 2900g/mol etc..
Preferably, the hydroxyl value of the superbrnaching end-hydroxy polyester be 500~600mg KOH/g, such as 505mg KOH/g,
510mg KOH/g, 520mg KOH/g, 540mg KOH/g, 550mg KOH/g, 570mg KOH/g, 580mg KOH/g or
590mg KOH/g etc..
Preferably, the hydroxyl moles of the superbrnaching end-hydroxy polyester be 4~25mol, such as 5mol, 7mol, 9mol,
10mol, 12mol, 15mol, 18mol, 20mol, 21mol or 22mol etc..
Highly-branched polymers in powder paint compositions of the present invention have unique tufted structure, molecule knot
The dissaving structure of structure makes its internal formation cavity, can be wrapped in it in conjunction with low surface energy auxiliary agent and by low surface energy auxiliary agent
In branched structure, composite construction is formed.The highly-branched polymers can promote matrix to melt in powder paint compositions
Mobility under state, while driving low surface energy auxiliary agent to float up to surface of the paint film, and then react with Isocyanates curing agent
Solidification, realizes the low-surface-energy of surface covering, and coating is made to have dirt-resistant and anti-graffiti characteristic.
Preferably, the Isocyanates curing agent is inner sealing type polyisocyanates.
Preferably, preparing in raw material for the powder paint compositions further includes 0.1~2 parts by weight (such as 0.2 weight
Part, 0.4 parts by weight, 0.6 parts by weight, 0.8 parts by weight, 1 parts by weight, 1.3 parts by weight, 1.5 parts by weight, 1.7 parts by weight or 1.9 weights
Measure part etc.) nanofiller.
Preferably, the nanofiller is selected from nano aluminium oxide, nano-titanium dioxide, nano silica, nano oxidized
In magnesium or nano zine oxide any one or at least two combination.
Preferably, the partial size of the nanofiller be 30~200nm, such as 40nm, 60nm, 80nm, 100nm, 120nm,
140nm, 150nm, 170nm or 190nm etc., further preferably 50~120nm.
Nanofiller can promote the ir-absorbance of powder paint compositions in the curing process in the present invention, facilitate
Realize the fast low temperature cure of paint film.
Preferably, preparing in raw material for the powder paint compositions further includes 0.5~2 parts by weight (such as 0.6 weight
Part, 0.8 parts by weight, 1 parts by weight, 1.3 parts by weight, 1.5 parts by weight, 1.7 parts by weight or 1.9 parts by weight etc.) curing accelerator.
Preferably, the curing accelerator be selected from imidazoles, imdazole derivatives, tertiary ammonium salt, quaternary ammonium salt, tetraalkyl phosphonium carboxylate's ammonium or
In dibutyl tin dilaurate any one or at least two combination.
Preferably, preparing in raw material for the powder paint compositions further includes 5~30 parts by weight (such as 7 parts by weight, 9
Parts by weight, 10 parts by weight, 13 parts by weight, 15 parts by weight, 18 parts by weight, 20 parts by weight, 23 parts by weight, 25 parts by weight, 27 weight
Part or 29 parts by weight etc.) pigments and fillers.
Preferably, the pigments and fillers are pigment and/or filler.
Preferably, the pigment is selected from titanium dioxide, iron oxide red, ultramarine, iron oxide yellow, any one in phthalocyanine blue or dark green
Kind or at least two combination.
Preferably, the filler in barium sulfate, wax powder, silicon powder or the mica powder any one or at least two
Combination.
Preferably, preparing in raw material for the powder paint compositions further includes 0.2~1 parts by weight (such as 0.3 weight
Part, 0.5 parts by weight, 0.7 parts by weight, 0.8 parts by weight or 0.9 parts by weight etc.) levelling agent.
Preferably, the levelling agent is polyacrylate levelling agent.
Preferably, preparing in raw material for the powder paint compositions further includes 0.1~0.5 parts by weight (such as 0.2 weight
Part, 0.3 parts by weight or 0.4 parts by weight etc.) degasser.
Preferably, the degasser is styrax.
Preferably, preparing in raw material for the powder paint compositions further includes 0.2~2 parts by weight (such as 0.3 weight
Part, 0.5 parts by weight, 0.8 parts by weight, 1 parts by weight, 1.3 parts by weight, 1.5 parts by weight, 1.7 parts by weight or 1.9 parts by weight etc.) profit
Hygroscopic water powder.
Preferably, the partial size of the powder paint compositions is 20~80 μm, such as 22 μm, 25 μm, 28 μm, 30 μm, 35 μ
M, 40 μm, 45 μm, 50 μm, 55 μm, 60 μm, 65 μm, 70 μm, 75 μm or 79 μm etc..
Preferably, the raw material for preparing of the powder paint compositions includes following ingredient:
Wherein, the terminal carboxyl polyester resin is the mixture of high acid value polyester resin and low acid value polyester resin, and institute
The mass ratio for stating high acid value polyester resin and low acid value polyester resin is 1:(4~9).
On the other hand, the present invention provides a kind of preparation method of powder paint compositions as described above, the preparation side
Method the following steps are included:
(1) highly-branched polymers and low surface energy auxiliary agent are mixed, dispersion, obtains mixture；
(2) mixture for obtaining step (1) and epoxy resin, terminal carboxyl polyester resin and Isocyanates curing agent
Mixing squeezes out, and obtains prefabricated material；
(3) it by prefabricated material tabletting that step (2) obtains and smashes, obtains the powder paint compositions.
Preferably, step (1) dispersion is carried out by high speed disperser.
Preferably, the rate of dispersion of the high speed disperser be 500~2000 turns, such as 600 turns, 800 turns, 1000 turns,
1200 turns, 1400 turns, 1500 turns, 1700 turns or 1900 turns etc..
Preferably, the time of step (1) described dispersion be 2~10min, such as 3min, 4min, 5min, 6min, 7min,
8min or 9min etc..
Preferably, step (2) is described is extruded through extruder progress.
Preferably, the temperature of step (2) described extrusion be 80~110 DEG C, such as 80 DEG C, 82 DEG C, 85 DEG C, 88 DEG C, 90 DEG C,
92 DEG C, 95 DEG C, 98 DEG C, 100 DEG C, 102 DEG C, 105 DEG C, 108 DEG C or 110 DEG C etc..
Preferably, described crush to be crushed to partial size of step (3) is 20~80 μm, for example, 22 μm, 25 μm, 28 μm, 30 μm,
35 μm, 40 μm, 45 μm, 50 μm, 55 μm, 60 μm, 65 μm, 70 μm, 75 μm or 79 μm etc..
Preferably, the preparation method specifically includes the following steps:
(1) highly-branched polymers and low surface energy auxiliary agent are mixed, the speed with high speed disperser at 500~2000 turns
2~10min of lower dispersion, obtains mixture；
(2) by mixture that step (1) obtains and epoxy resin, terminal carboxyl polyester resin, Isocyanates curing agent, receive
It is rice filler, curing accelerator, pigments and fillers, levelling agent, degasser and wetting dispersing agent mixing, broken, with extruder 80~
It is squeezed out under the conditions of 110 DEG C, obtains prefabricated material；
(3) prefabricated material tabletting, cooling, the smashing to partial size obtained step (2) is 20~80 μm, sieves, and is obtained described
Powder paint compositions.
Powder paint compositions of the present invention are needed first in the preparation by low surface energy auxiliary agent and highly-branched polymers
It is sufficiently mixed, is uniformly dispersed, be then blended, be crushed, squeeze out with other components again；The preparation sequence is to make low-surface-energy
Auxiliary agent is first combined with highly-branched polymers, and in film forming, highly-branched polymers can more efficiently promote low-surface-energy
Auxiliary agent floats up to film coated surface.
On the other hand, the present invention provides a kind of heatsensitive substrates coating, and the heatsensitive substrates coating includes thermal sensitivity base
Material and its film on surface, the raw material of the film are powder paint compositions as described above.
On the other hand, the present invention provides a kind of preparation method of heatsensitive substrates coating as described above, the preparation side
Method the following steps are included:
The powder paint compositions are coated on heatsensitive substrates using high-pressure electrostatic method or fluidized bed process, are passed through
Medium-wave infrared furnace is solidified, and the heatsensitive substrates coating is obtained.
Preferably, the cured power is 5~30kW/m2, such as 6kW/m2、8kW/m2、10kW/m2、12kW/m2、
14kW/m2、15kW/m2、17kW/m2、20kW/m2、23kW/m2、25kW/m2、27kW/m2Or 29kW/m2Deng.
Preferably, the cured time be 3~10min, such as 4min, 5min, 6min, 7min, 8min or 9min etc.,
Further preferably 3~5min.
Compared with the existing technology, the invention has the following advantages:
Phase interworking of the powder paint compositions provided by the invention by the design and each component of component under special ratios
It closes, so that the powder paint compositions rapid curing can be formed a film at low temperature, the curing degree of paint film is resistance to molten greater than 98% after solidification
Agent wiping number reaches 200 times or more, is not less than 100 degree with the contact angle of water, antigraffiti properties are 1 grade, and anti-stick patch property is less than
0.1N/mm.Powder paint compositions of the present invention are highly applicable to the heatsensitive substrates such as timber, glass, paper and plastics
The coating on surface, the hardness of paint film is high after solidification, flexibility is good, crosslink density is high, has excellent anti-graffiti property and dirt-resistant
Property.
Specific embodiment
The technical scheme of the invention is further explained by means of specific implementation.Those skilled in the art should be bright
, the described embodiments are merely helpful in understanding the present invention, should not be regarded as a specific limitation of the invention.
Examples 1 to 8
A kind of powder paint compositions, the ingredient for preparing raw material is as shown in table 1, and the unit of the ingredient is " weight
Part ".
Table 1
Wherein, bisphenol A type epoxy resin is the good E12 (604) of Anhui U.S., epoxide equivalent 830；Novolac epoxy resin
Epoxide equivalent is 225 (Aralaite ECN 9669)；Aliphatic epoxy resin is aliphatic glycidyl ether based epoxy resin,
Epoxide equivalent is 330 (Tao Shi DER732)；The acid value of high acid value polyester resin is 70mg KOH/g (Crylcoat 1501)；It is low
The acid value of acid value polyester resin is 35mg KOH/g (Crylcoat 04432)；The number-average molecular weight of superbrnaching end-hydroxy polyester is
1100g/mol, hydroxyl value are 580mg KOH/g (SeHBP H102)；Low surface energy auxiliary agent is organic-silicon-modified hydroxy acrylate
(WE-9610D)；Isocyanates curing agent is inner sealing type polyisocyanates (VESTAGON 1321)；Nano aluminium oxide is put down
Equal partial size is 80nm；Levelling agent is esters of acrylic acid levelling agent (Ningbo South Sea chemistry GLP588)；Degasser is styrax；Wetting
Dispersing agent is GLP701.
The preparation method is as follows:
(1) highly-branched polymers and low surface energy auxiliary agent are mixed, is divided under 1000 turns of speed with high speed disperser
5min is dissipated, mixture is obtained；
(2) mixture that step (1) obtains is mixed with remaining component, is broken, squeezed under the conditions of 100 DEG C with extruder
Out, prefabricated material is obtained；
(3) prefabricated material tabletting, cooling, the smashing to partial size obtained step (2) is 20~80 μm, sieves, and is obtained described
Powder paint compositions.
Embodiment 9
The present embodiment and the difference of embodiment 4 are that low surface energy auxiliary agent is that (Hua Tongrui's fluorine richness hydroxy acrylate speeds
A89)。
Comparative example 1
The difference of this comparative example and embodiment 4 is, does not add superbrnaching end-hydroxy polyester.
Comparative example 2
The difference of this comparative example and embodiment 4 is, does not add superbrnaching end-hydroxy polyester, the addition of low surface energy auxiliary agent
Amount is 10 parts by weight.
Comparative example 3
The difference of this comparative example and embodiment 4 is, does not add high acid value polyester resin, the addition of low acid value polyester resin
Amount is 35 parts by weight.
Comparative example 4
The difference of this comparative example and embodiment 4 is, does not add low surface energy auxiliary agent.
Comparative example 5
The difference of this comparative example and embodiment 4 is that the additive amount of superbrnaching end-hydroxy polyester is 11 parts by weight.
Comparative example 6
The difference of this comparative example and embodiment 4 is that the additive amount of superbrnaching end-hydroxy polyester is 0.3 parts by weight.
Application examples
A kind of coating of powdery paints, preparation method are as follows:
Using high-pressure electrostatic method by the powder paint compositions provided in Examples 1 to 9, comparative example 1~6 be coated on by
It on the substrate of surface cleaning processing, is subsequently placed in medium-wave infrared furnace (Sweden TRIAB), setting solidification power is 10kW/m2Gu
It is taken out after changing 4min, obtains the coating that average dry film thickness is 80 μm.
Above-mentioned substrate is selected according to the difference of test item, evaluates the appearance property (levelability, glossiness) of paint film
The heatsensitive substrates such as timber, glass can be used, evaluating the mechanical performances such as the solvent resistant wiping of film, adhesive force, hardness need to be according to
Corresponding testing standard selects substrate.
Paint film property test:
(1) Coated Surface Temperature: with the surface temperature of thermal infrared imager real-time monitoring solidification process floating coat, temperature is got over
Height shows that the ir-absorbance of powdery paints is higher；
(2) curing of coatings degree: curing of coatings degree is a, and the total amount of heat that uncured powder coating discharges when being fully cured is Δ
H0(J/g), remaining reaction heat is Δ H when not being fully curedR(J/g), wherein Δ H0(J/g)、ΔHR(J/g) it is surveyed by DSC
Examination obtains, curing degree a=(Δ H0-ΔHR)/ΔH0；
(3) anti-graffiti property: being tested according to the regulation of JGT 304-2011 standard, respectively test paint film for prepared Chinese ink,
Permanent pen and the antigraffiti properties of acrylic acid spray painting；1 grade indicates to be removed with doing lint-free cotton, and 2 grades indicate in 1%
The aqueous weak cleaning agent of property can be removed, and 3 grades of expression citrus based cleaning agents can be removed, and 4 grades of expression dehydrated alcohols can be removed, " no
Can remove " indicate the discoloration of coating loss of gloss or damage after above-mentioned four kinds of cleaning materials cannot be removed or be cleaned；
(4) it contact angle: using the contact angle of contact angle measurement (KRUSS DSA100) test surface of the paint film, tests respectively
Water droplet contact angle and oil droplet (olive oil) contact angle, contact angle is bigger, and the anti-stain characteristic for representing paint film is better；
(5) hardness: according to the pencil hardness of the regulation test paint film of GB/T 6739-2006 standard；
(6) solvent resistance: being tested according to instrument wipe method as defined in GB/T 23989-2009 standard, wipes reagent
For butanone；
(7) 180 ° of peel strength tests anti-stick patch: are carried out according to the standard regulation of GB/T 2792-2004；
(8) it flexibility: is tested according to the standard regulation of GB/T 1731-1993；
(9) adhesive force: according to stroke hundred lattice adhesive force of the standard testing paint film of GB/T 9286-1998.
Performance after the film forming for the powder paint compositions that testing example 1~9 provides according to the method described above, as a result such as table
Shown in 2:
Table 2
Performance after the film forming for the powder paint compositions that test comparison example 1~6 provides according to the method described above, as a result such as table
Shown in 3:
Table 3
It is available from the data of table 2, when powder paint compositions film-forming provided by the invention ir-absorbance it is high,
Curing rate is fast, obtained paint film hardness with higher, flexibility, adhesive force and solvent resistance and excellent anti-graffiti
Property and anti-stain characteristic.Compared to embodiment 4, using being adopted in the bisphenol A type epoxy resin of single kind, embodiment 8 in embodiment 7
With single low acid value polyester resin, the crosslink density that will lead to paint film is reduced, thus make the hardness of paint film, solvent resistance and
Flexibility is declined.
Contrast table 2 and the data of table 3 are available, when not containing highly-branched polymers in powder paint compositions
(comparative example 1), the curing degree of paint film, surface temperature, hardness, flexibility, adhesive force, solvent resistance, anti-graffiti property and anti-is stained with
Dirt decreased significantly, and illustrate that highly-branched polymers not only promote low surface energy auxiliary agent to float up to surface of the paint film, facilitate
The reduction of surface of the paint film energy, and react as one of cross-linking component and curing agent, the friendship after increasing powdery paints film forming
Join density, to facilitate the promotion of hardness and solvent resistance.
(the comparison when not containing highly-branched polymers in powder paint compositions and increase the dosage of low surface energy auxiliary agent
Example 2), the anti-graffiti property and contact angle of paint film are promoted, but solvent resistance and mechanical performance are still bad, illustrate in the present invention
The anti-graffiti property and anti-stain characteristic of paint film are that highly-branched polymers and low surface energy auxiliary agent are coordinated as a result, single raising
The dosage of low surface energy auxiliary agent facilitates the reduction of surface of the paint film energy, but does not have to overall targets such as the patience of paint film, mechanical performances
There is obvious benefit.
When terminal carboxyl polyester resin in powder paint compositions dosage be lower than the framework of the present definition (comparative example 3),
Curing degree, hardness, flexibility, adhesive force, solvent resistance, anti-graffiti property and the anti-stain characteristic of paint film decreased significantly, and say
A large amount of cross-linking reaction sites that terminal carboxyl polyester resin provides in the bright present invention are the key factor for improving paint film crosslink density, end
The too low crosslink density decline for directly resulting in paint film of carboxyl polyester resin content, to influence the mechanical performance and solvent resistant of paint film
Property；The reduction of hardness further affects the anti-graffiti property of paint film and anti-stain characteristic.
When not containing low surface energy auxiliary agent in powder paint compositions (comparative example 4), the surface of paint film can be higher, anti-painting
Crow property and anti-stain characteristic are bad.
When the dosage of highly-branched polymers in powder paint compositions is lower than the framework of the present definition, dosage mistake
High (comparative example 5) then can make paint film firmly crisp, and flexibility is not good enough；Dosage too low (comparative example 6), which does not have then, significantly promotes low table
Face energy auxiliary agent floats and the effect of increase crosslink density, can not effectively improve paint film mechanical performance and anti-graffiti anti-stain characteristic
Energy.
The Applicant declares that the present invention is explained by the above embodiments powder paint compositions and its preparation side of the invention
Method and application, but the present invention is not limited to the above embodiments, that is, does not mean that the present invention must rely on above-described embodiment ability
Implement.It should be clear to those skilled in the art, any improvement in the present invention, to each raw material of product of the present invention etc.
Effect replacement and addition, the selection of concrete mode of auxiliary element etc., all of which fall within the scope of protection and disclosure of the present invention.
Claims (10)
1. a kind of powder paint compositions, which is characterized in that the raw material for preparing of the powder paint compositions includes following ingredient:
2. powder paint compositions according to claim 1, which is characterized in that the epoxy resin includes following ingredient:
40~60 parts by weight of bisphenol-type epoxy resin
10~20 parts by weight of novolac epoxy resin
1~10 parts by weight of aliphatic epoxy resin；
Preferably, the bisphenol-type epoxy resin is selected from bisphenol A type epoxy resin, bisphenol-s epoxy resin, bisphenol F type epoxy
In resin, bisphenol-A epoxy resin or tetrabormated bisphenol A type epoxy resin any one or at least two combination；
Preferably, the novolac epoxy resin is linear phenolic epoxy resin.
3. powder paint compositions according to claim 1 or 2, which is characterized in that the terminal carboxyl polyester resin is height
The mixture of acid value polyester resin and low acid value polyester resin；
Preferably, the mass ratio of the high acid value polyester resin and low acid value polyester resin is 1:(4~9)；
Preferably, the acid value of the high acid value polyester resin is 70~90mg KOH/g；
Preferably, the acid value of the low acid value polyester resin is 10~40mg KOH/g.
4. described in any item powder paint compositions according to claim 1~3, which is characterized in that the low surface energy auxiliary agent
Dosage be 0.2~3 parts by weight；
Preferably, the low surface energy auxiliary agent is organosilicon auxiliary agent and/or fluorine auxiliary agent；
Preferably, the organosilicon auxiliary agent is that organic-silicon-modified hydroxy acrylate, hydroxy silicon oil or organic-silicon-modified hydroxyl are poly-
In ester resin any one or at least two combination；
Preferably, the fluorine auxiliary agent is fluorine richness hydroxy acrylate；
Preferably, the highly-branched polymers be dendritic or dissaving polymer, it is further preferably hyperbranched
Polymer；
Preferably, the dissaving polymer is superbrnaching end-hydroxy polyester；
Preferably, the number-average molecular weight of the superbrnaching end-hydroxy polyester is 500~3000g/mol；
Preferably, the hydroxyl value of the superbrnaching end-hydroxy polyester is 500~600mg KOH/g；
Preferably, the hydroxyl moles of the superbrnaching end-hydroxy polyester are 4~25mol.
5. powder paint compositions according to any one of claims 1 to 4, which is characterized in that the isocyanates is solid
Agent is inner sealing type polyisocyanates；
Preferably, preparing in raw material for the powder paint compositions further includes 0.1~2 parts by weight nanofiller；
Preferably, the nanofiller be selected from nano aluminium oxide, nano-titanium dioxide, nano silica, nano magnesia or
In nano zine oxide any one or at least two combination；
Preferably, the partial size of the nanofiller is 30~200nm, further preferably 50~120nm；
Preferably, preparing in raw material for the powder paint compositions further includes 0.5~2 parts by weight curing accelerator；
Preferably, the curing accelerator is selected from imidazoles, imdazole derivatives, tertiary ammonium salt, quaternary ammonium salt, tetraalkyl phosphonium carboxylate's ammonium or February
In dilaurylate any one or at least two combination；
Preferably, preparing in raw material for the powder paint compositions further includes 5~30 parts by weight pigments and fillers；
Preferably, the pigments and fillers are pigment and/or filler；
Preferably, the pigment is selected from titanium dioxide, iron oxide red, ultramarine, iron oxide yellow, in phthalocyanine blue or dark green any one or
At least two combination；
Preferably, the filler in barium sulfate, wax powder, silicon powder or mica powder any one or at least two group
It closes；
Preferably, preparing in raw material for the powder paint compositions further includes 0.2~1 parts by weight levelling agent；
Preferably, the levelling agent is polyacrylate levelling agent；
Preferably, preparing in raw material for the powder paint compositions further includes 0.1~0.5 parts by weight degasser；
Preferably, the degasser is styrax；
Preferably, preparing in raw material for the powder paint compositions further includes 0.2~2 parts by weight wetting dispersing agent；
Preferably, the partial size of the powder paint compositions is 20~80 μm；
Preferably, the raw material for preparing of the powder paint compositions includes following ingredient:
Wherein, the terminal carboxyl polyester resin is the mixture of high acid value polyester resin and low acid value polyester resin, and the height
The mass ratio of acid value polyester resin and low acid value polyester resin is 1:(4~9).
6. a kind of preparation method of powder paint compositions as claimed in any one of claims 1 to 5, which is characterized in that described
Preparation method the following steps are included:
(1) highly-branched polymers and low surface energy auxiliary agent are mixed, dispersion, obtains mixture；
(2) mixture that step (1) obtains is mixed with epoxy resin, terminal carboxyl polyester resin and Isocyanates curing agent
It squeezes out, obtains prefabricated material；
(3) it by prefabricated material tabletting that step (2) obtains and smashes, obtains the powder paint compositions.
7. preparation method according to claim 6, which is characterized in that step (1) it is described dispersion by high speed disperser into
Row；
Preferably, the rate of dispersion of the high speed disperser is 500~2000 turns；
Preferably, the time of step (1) described dispersion is 2~10min；
Preferably, step (2) is described is extruded through extruder progress；
Preferably, the temperature of step (2) described extrusion is 80~110 DEG C；
Preferably, described crush to be crushed to partial size of step (3) is 20~80 μm；
Preferably, the preparation method specifically includes the following steps:
(1) highly-branched polymers and low surface energy auxiliary agent are mixed, is divided under 500~2000 turns of speed with high speed disperser
2~10min is dissipated, mixture is obtained；
(2) mixture that step (1) obtains is filled out with epoxy resin, terminal carboxyl polyester resin, Isocyanates curing agent, nanometer
Material, curing accelerator, pigments and fillers, levelling agent, degasser and wetting dispersing agent mixing are crushed, with extruder at 80~110 DEG C
Under the conditions of squeeze out, obtain prefabricated material；
(3) prefabricated material tabletting, cooling, the smashing to partial size obtained step (2) is 20~80 μm, sieves, and obtains the powder
Coating composition.
8. a kind of heatsensitive substrates coating, which is characterized in that the heatsensitive substrates coating includes heatsensitive substrates and its surface
Film, the raw material of the film is powder paint compositions as claimed in any one of claims 1 to 5.
9. a kind of preparation method of heatsensitive substrates coating as claimed in claim 8, which is characterized in that the preparation method packet
Include following steps:
The powder paint compositions are coated on heatsensitive substrates using high-pressure electrostatic method or fluidized bed process, pass through medium wave
Infra-red furnace is solidified, and the heatsensitive substrates coating is obtained.
10. preparation method according to claim 9, which is characterized in that the cured power is 5~30kW/m2；
Preferably, the cured time is 3~10min, further preferably 3~5min.
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