CN110330870A - A kind of powdery paints and preparation method - Google Patents
A kind of powdery paints and preparation method Download PDFInfo
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- CN110330870A CN110330870A CN201910580817.3A CN201910580817A CN110330870A CN 110330870 A CN110330870 A CN 110330870A CN 201910580817 A CN201910580817 A CN 201910580817A CN 110330870 A CN110330870 A CN 110330870A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/14—Methyl esters, e.g. methyl (meth)acrylate
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/02—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds
- C08G63/12—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds derived from polycarboxylic acids and polyhydroxy compounds
- C08G63/16—Dicarboxylic acids and dihydroxy compounds
- C08G63/18—Dicarboxylic acids and dihydroxy compounds the acids or hydroxy compounds containing carbocyclic rings
- C08G63/181—Acids containing aromatic rings
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/02—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds
- C08G63/12—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds derived from polycarboxylic acids and polyhydroxy compounds
- C08G63/16—Dicarboxylic acids and dihydroxy compounds
- C08G63/20—Polyesters having been prepared in the presence of compounds having one reactive group or more than two reactive groups
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/78—Preparation processes
- C08G63/785—Preparation processes characterised by the apparatus used
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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
- C09D167/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- 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
- C09D5/031—Powdery paints characterised by particle size or shape
-
- 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
-
- 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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
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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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- 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
- C08K2201/002—Physical properties
- C08K2201/003—Additives being defined by their diameter
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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
Abstract
The invention discloses a kind of powdery paints, it is prepared from the following raw materials in parts by weight: 400-500 parts of neopentyl glycol, 700-800 parts of isophthalic acid, three sad 6 parts of normal-butyl tin, Isosorbide-5-Nitrae -500-600 parts of cyclohexane dimethanol, 10-20 parts of trimethylolpropane, 500-600 parts of adipic acid, 1 part of phosphorous acid, 100 parts of n-butyl acetate, 1 part of tert butyl peroxy benzoate, 24 parts of styrene, 26 parts of benzyl propionic acid, 50 parts of methylpropionic acid methyl esters.Described three sad 6 parts of tin of normal-butyls are divided into three sad 2.5 parts of normal-butyl tin, 2.5 parts of three sad normal-butyl tin and three sad 1 part of tin of normal-butyls.The powdery paints have corner on powder it is uniform, solidification after paint film defect be easy cover and the lower effect of condition of cure.
Description
Technical field
Invention is related to powder coating technology field, specially a kind of powdery paints and preparation method.
Background technique
Powdery paints is the form entirely different with general coating, it is existing for state with attritive powder.Due to not
Using solvent, so referred to as powdery paints.The main feature of powdery paints has: having harmless, high efficiency, saves resource and environmental protection
Feature.It has two major classes: thermoplastic powder coating and thermosetting powder coating.Thermoplastic powder coating be by thermoplastic resin,
Pigment, filler, plasticizer and stabilizer etc. are at being grouped as.Thermoplastic powder coating includes: polyethylene, polypropylene, polyester, gathers
Vinyl chloride, chlorinated polyether, polyamide-based, cellulose-based, Polyester etc..Thermosetting powder coating includes: epoxy resin, ring
Oxygen-Polyester, Polyester, polyurethane series, acrylic resin etc..
Current thermoplastic powder coating and thermosetting powder coating, exist powder on corner it is inhomogenous, solidification after film
Defect be difficult to conceal with the higher problem of condition of cure, and its preparation process exist be easy to cause many by-products to be entrained in powder
In coating, the problem of influencing the service performance of powdery paints.
Summary of the invention
Invention is designed to provide a kind of powdery paints and preparation method, to solve mentioned above in the background art ask
Topic.
To achieve the above object, invention provides the following technical solutions: a kind of powdery paints, by the original of following parts by weight
Material is made: 400-500 parts of neopentyl glycol, 700-800 parts of isophthalic acid, three sad 6 parts of normal-butyl tin, 1,4- cyclohexane dimethanol
500-600 parts, 10-20 parts of trimethylolpropane, 500-600 parts of adipic acid, 1 part of phosphorous acid, 100 parts of n-butyl acetate, tertiary fourth
1 part of base peroxide benzoate, 24 parts of styrene, 26 parts of benzyl propionic acid, 50 parts of methylpropionic acid methyl esters.
Preferably, described three sad 6 parts of tin of normal-butyls are divided into three sad 2.5 parts of normal-butyl tin, three sad normal-butyl tin 2.5
Part and three sad 1 part of tin of normal-butyls.
Preferably, the powdery paints further includes 40-50 parts of triglycidyl isocyanurate.
Preferably, the powdery paints further includes 20-30 microns of average grain diameter of 200-300 parts of barium sulfate and average grain diameter
200-300 parts of 20-30 microns of calcium carbonate.
Preferably, the powdery paints further includes 2-3 parts and optical brightener 1-3 parts of levelling agent.
Preferably, the powdery paints also wraps brilliant by cinnabar, laterite, realgar, peacock green, powdered whiting, wollastonite, weight
One of mountain flour, talcum powder, mica powder and kaolin or a variety of 20-30 microns of average grain diameter mixed of natural dyes.
A kind of preparation method of powdery paints, specifically includes the following steps:
Step 1: taking 450 parts of neopentyl glycols to be added in thermocouple reaction kettle, uniform stirring in the environment of being full of nitrogen
And 135 DEG C are heated to, 750 parts of isophthalic acids and 2.5 part of three sad normal-butyl tin are added, 240 DEG C are progressively heated at, from 190 DEG C
It rises, water is distilled out from reactor, keeps 240 DEG C of reaction 3h, and the product acid value finally obtained is 38mgKOH/g, and hydroxyl value is
4mgKOH/g, viscosity are the product of 2200mpa.s；
Step 2: 550 parts of 1,4- cyclohexane dimethanols, 15 parts of trimethylolpropanes, 550 parts of adipic acids and 2.5 part three are taken
Sad normal-butyl tin is added in thermocouple reaction kettle, uniform stirring and is heated to 135 DEG C in the environment of being full of nitrogen, gradually
230 DEG C are heated to, continues to and 1 part of phosphorous acid and 1 part of three sad normal-butyl tin is added after water is distilled completely, and is anti-toward thermocouple
It answers in kettle gradually plus the vacuum of 7kpa, in 230 DEG C of at a temperature of sustained response 5h, 26mgKOH/g is obtained, hydroxyl value is
4mgKOH/g, viscosity are the product of 6800mpa.s；
Step 3: taking 100 parts of n-butyl acetates to be added in thermocouple reaction kettle, uniform stirring and continuous heating, simultaneously
It is purged using nitrogen, when temperature is promoted to 130 DEG C, is added by 1 part of tert butyl peroxy benzoate and 22 parts of styrene
Mixture after sustained response 3.5h, is added 24 parts of styrene, 26 parts of benzyl propionic acid, 50 parts of methylpropionic acid methyl esters, maintains reaction
Time obtains the product that viscosity is 1800mpa.s after being 1.5h；
Step 4: will be Step 1: the mixture obtained in step 2 and step 3 is added to a thermocouple reaction kettle
In, 240 DEG C of lasting 30-60min are heated to, is added after three kinds of mixing are all melted and stirred and is separately added into 45 parts
Triglycidyl isocyanurate, 250 parts of barium sulfate, 250 parts of calcium carbonate, 2.5 parts of levelling agents, 1.5 parts of optical brighteners and with it is total
The comparable natural dye of mixing quality carries out being sufficiently mixed stirring, is then melted and is homogenized with double screw extruder, is added after cooling
It grinds in grinder, finally powder is sieved according to Particle size requirements, obtain powdery paints.
Preferably, the thermocouple reaction kettle is to enter equipped with blender, the distillation column being connected with water cooled condenser, nitrogen
The thermocouple reaction kettle that mouth is connected with thermoregulator.
Compared with prior art, advantageous effect of the invention is: the powdery paints and preparation method, passes through new the penta 2 of setting
The sad normal-butyl tin of alcohol, isophthalic acid and three prepares amorphous polyester, by the way that Isosorbide-5-Nitrae-cyclohexane dimethanol, trihydroxy methyl third is arranged
Alkane, adipic acid, three sad normal-butyl tin, phosphorous acid and three sad normal-butyl tin prepare semicrystalline polyester, just by setting acetic acid
It is total that butyl ester, tert butyl peroxy benzoate and styrene, styrene, benzyl propionic acid and methylpropionic acid methyl esters prepare acrylic acid
Polymers, amorphous polyester therein have polar group, and powder utilization is higher, can be inhomogenous with powder on effective solution corner
The problem of；The metal adhesion of semicrystalline polyester therein is strong, and condition of cure requirement is low, can effectively reduce condition of cure；
Acrylic copolymer therein dissolves under spraying temperature, and freezing film when cooling need to only heat fusing, levelling, cooling or extraction
Freezing film is taken, paint film defect is difficult to conceal after solving the problems, such as solidification；And preparation, the semicrystalline polyester of amorphous polyester
Preparation and acrylic copolymer preparation individually equipped with blender, be connected with water cooled condenser distillation column,
It is carried out in the thermocouple reaction kettle that nitrogen inlet is connected with thermoregulator, nitrogen gathers as protective gas in preparation process
It is mutually indepedent to close reaction, temperature-controllable is interference-free and free from the influence of the external environment, similarly in nothing in last mixing
The preparation of amorphous polyester, the preparation of semicrystalline polyester and the preparation of acrylic copolymer individually equipped in blender into
Row, instrument needed for entire process flow is few, and less input, and links independently carry out, and saves the time, improves preparation efficiency.
Specific embodiment
Below in conjunction with the embodiment of the present invention, technical scheme in the embodiment of the invention is clearly and completely described,
Obviously, described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based in the present invention
Embodiment, every other embodiment obtained by those of ordinary skill in the art without making creative efforts, all
Belong to the scope of protection of the invention.
Embodiment 1
A kind of powdery paints, is prepared from the following raw materials in parts by weight:
450 parts of neopentyl glycol, 750 parts of isophthalic acid, three sad 6 parts of normal-butyl tin, 550 parts of 1,4- cyclohexane dimethanol,
15 parts of trimethylolpropane, 550 parts of adipic acid, 1 part of phosphorous acid, 100 parts of n-butyl acetate, tert butyl peroxy benzoate 1
Part, 24 parts of styrene, 26 parts of benzyl propionic acid, 50 parts of methylpropionic acid methyl esters.Described three sad 6 parts of tin of normal-butyls are divided into three octanoic acids
2.5 parts of normal-butyl tin, 2.5 parts of three sad normal-butyl tin and three sad 1 part of tin of normal-butyls.The powdery paints further includes three epoxies
450 parts of propyl chlorinated isocyanurates.The powdery paints further includes 20-30 microns of average grain diameter of 250 parts of barium sulfate and average grain
250 parts of the calcium carbonate that 20-30 microns of diameter.The powdery paints further includes 2.5 parts and 2 parts of optical brightener of levelling agent.The powder applies
Material also packet is by cinnabar, laterite, realgar, peacock green, powdered whiting, wollastonite, blanc fixe, talcum powder, mica powder and kaolinite
One of soil or a variety of 20-30 microns of average grain diameter mixed of natural dyes.
A kind of preparation method of powdery paints, specifically includes the following steps:
Step 1: taking 450 parts of neopentyl glycols to be added in thermocouple reaction kettle, uniform stirring in the environment of being full of nitrogen
And 135 DEG C are heated to, 750 parts of isophthalic acids and 2.5 part of three sad normal-butyl tin are added, 240 DEG C are progressively heated at, from 190 DEG C
It rises, water is distilled out from reactor, keeps 240 DEG C of reaction 3h, and the product acid value finally obtained is 38mgKOH/g, and hydroxyl value is
4mgKOH/g, viscosity are the product of 2200mpa.s；
Step 2: 550 parts of 1,4- cyclohexane dimethanols, 15 parts of trimethylolpropanes, 550 parts of adipic acids and 2.5 part three are taken
Sad normal-butyl tin is added in thermocouple reaction kettle, uniform stirring and is heated to 135 DEG C in the environment of being full of nitrogen, gradually
230 DEG C are heated to, continues to and 1 part of phosphorous acid and 1 part of three sad normal-butyl tin is added after water is distilled completely, and is anti-toward thermocouple
It answers in kettle gradually plus the vacuum of 7kpa, in 230 DEG C of at a temperature of sustained response 5h, 26mgKOH/g is obtained, hydroxyl value is
4mgKOH/g, viscosity are the product of 6800mpa.s；
Step 3: taking 100 parts of n-butyl acetates to be added in thermocouple reaction kettle, uniform stirring and continuous heating, simultaneously
It is purged using nitrogen, when temperature is promoted to 130 DEG C, is added by 1 part of tert butyl peroxy benzoate and 22 parts of styrene
Mixture after sustained response 3.5h, is added 24 parts of styrene, 26 parts of benzyl propionic acid, 50 parts of methylpropionic acid methyl esters, maintains reaction
Time obtains the product that viscosity is 1800mpa.s after being 1.5h；
Step 4: will be Step 1: the mixture obtained in step 2 and step 3 is added to a thermocouple reaction kettle
In, 240 DEG C of lasting 30-60min are heated to, is added after three kinds of mixing are all melted and stirred and is separately added into 45 parts
Triglycidyl isocyanurate, 250 parts of barium sulfate, 250 parts of calcium carbonate, 2.5 parts of levelling agents, 1.5 parts of optical brighteners and with it is total
The comparable natural dye of mixing quality carries out being sufficiently mixed stirring, is then melted and is homogenized with double screw extruder, is added after cooling
It grinds in grinder, finally powder is sieved according to Particle size requirements, obtain powdery paints.
The thermocouple reaction kettle is equipped with blender, the distillation column being connected with water cooled condenser, nitrogen inlet and temperature
The thermocouple reaction kettle that degree adjuster is connected.
Embodiment 2
A kind of powdery paints, is prepared from the following raw materials in parts by weight: 400 parts of neopentyl glycol, 700 parts of isophthalic acid,
Three sad 6 parts of normal-butyl tin, 500 parts of 1,4- cyclohexane dimethanol, 10 parts of trimethylolpropane, 500 parts of adipic acid, phosphorous acid 1
Part, 100 parts of n-butyl acetate, 1 part of tert butyl peroxy benzoate, 24 parts of styrene, 26 parts of benzyl propionic acid, methylpropanoic acid
50 parts of methyl esters.Three sad 6 parts of tin of the normal-butyls are divided into three sad 2.5 parts of normal-butyl tin, 2.5 parts of three sad normal-butyl tin and three
1 part of sad normal-butyl tin.The powdery paints further includes 40 parts of triglycidyl isocyanurate.The powdery paints further includes
200 parts of calcium carbonate of 200 parts and average grain diameter 20-30 microns of the barium sulfate that 20-30 microns of average grain diameter.The powdery paints is also
Including 2 parts and 1 part of optical brightener of levelling agent.The powdery paints also wrap by cinnabar, laterite, realgar, peacock green, powdered whiting,
One of wollastonite, blanc fixe, talcum powder, mica powder and kaolin are mixed 20-30 microns of average grain diameter a variety of
Natural dye.
A kind of preparation method of powdery paints, specifically includes the following steps:
Step 1: taking 400 parts of neopentyl glycols to be added in thermocouple reaction kettle, uniform stirring in the environment of being full of nitrogen
And 135 DEG C are heated to, 700 parts of isophthalic acids and 2.5 part of three sad normal-butyl tin are added, 240 DEG C are progressively heated at, from 190 DEG C
It rises, water is distilled out from reactor, keeps 240 DEG C of reaction 3h, and the product acid value finally obtained is 38mgKOH/g, and hydroxyl value is
4mgKOH/g, viscosity are the product of 2200mpa.s；
Step 2: 500 parts of 1,4- cyclohexane dimethanols, 10 parts of trimethylolpropanes, 500 parts of adipic acids and 2.5 part three are taken
Sad normal-butyl tin is added in thermocouple reaction kettle, uniform stirring and is heated to 135 DEG C in the environment of being full of nitrogen, gradually
230 DEG C are heated to, continues to and 1 part of phosphorous acid and 1 part of three sad normal-butyl tin is added after water is distilled completely, and is anti-toward thermocouple
It answers in kettle gradually plus the vacuum of 7kpa, in 230 DEG C of at a temperature of sustained response 5h, 26mgKOH/g is obtained, hydroxyl value is
4mgKOH/g, viscosity are the product of 6800mpa.s；
Step 3: taking 100 parts of n-butyl acetates to be added in thermocouple reaction kettle, uniform stirring and continuous heating, simultaneously
It is purged using nitrogen, when temperature is promoted to 130 DEG C, is added by 1 part of tert butyl peroxy benzoate and 22 parts of styrene
Mixture after sustained response 3.5h, is added 24 parts of styrene, 26 parts of benzyl propionic acid, 50 parts of methylpropionic acid methyl esters, maintains reaction
Time obtains the product that viscosity is 1800mpa.s after being 1.5h；
Step 4: will be Step 1: the mixture obtained in step 2 and step 3 is added to a thermocouple reaction kettle
In, 240 DEG C of lasting 30-60min are heated to, is added after three kinds of mixing are all melted and stirred and is separately added into 40 parts
Triglycidyl isocyanurate, 200 parts of barium sulfate, 200 parts of calcium carbonate, 2 parts of levelling agents, 1 part of optical brightener and with always mix
The comparable natural dye of quality carries out being sufficiently mixed stirring, is then melted and is homogenized with double screw extruder, and grinding is added after cooling
It grinds in machine, finally powder is sieved according to Particle size requirements, obtain powdery paints.
The thermocouple reaction kettle is equipped with blender, the distillation column being connected with water cooled condenser, nitrogen inlet and temperature
The thermocouple reaction kettle that degree adjuster is connected.
Embodiment 3
A kind of powdery paints, is prepared from the following raw materials in parts by weight: 500 parts of neopentyl glycol, 800 parts of isophthalic acid,
Three sad 6 parts of normal-butyl tin, 600 parts of 1,4- cyclohexane dimethanol, 20 parts of trimethylolpropane, 600 parts of adipic acid, phosphorous acid 1
Part, 100 parts of n-butyl acetate, 1 part of tert butyl peroxy benzoate, 24 parts of styrene, 26 parts of benzyl propionic acid, methylpropanoic acid
50 parts of methyl esters.Three sad 6 parts of tin of the normal-butyls are divided into three sad 2.5 parts of normal-butyl tin, 2.5 parts of three sad normal-butyl tin and three
1 part of sad normal-butyl tin.The powdery paints further includes 40-50 parts of triglycidyl isocyanurate.The powdery paints is also
Including 300 parts of calcium carbonate of 300 parts and average grain diameter 20-30 microns of barium sulfate of 20-30 microns of average grain diameter.The powder applies
Material further includes 3 parts and 3 parts of optical brightener of levelling agent.The powdery paints is also wrapped by cinnabar, laterite, realgar, peacock green, heavy carbonic acid
One of calcium, wollastonite, blanc fixe, talcum powder, mica powder and kaolin are mixed 20-30 microns of average grain diameter a variety of
Natural dye.
A kind of preparation method of powdery paints, specifically includes the following steps:
Step 1: taking 500 parts of neopentyl glycols to be added in thermocouple reaction kettle, uniform stirring in the environment of being full of nitrogen
And 135 DEG C are heated to, 800 parts of isophthalic acids and 2.5 part of three sad normal-butyl tin are added, 240 DEG C are progressively heated at, from 190 DEG C
It rises, water is distilled out from reactor, keeps 240 DEG C of reaction 3h, and the product acid value finally obtained is 38mgKOH/g, and hydroxyl value is
4mgKOH/g, viscosity are the product of 2200mpa.s；
Step 2: 600 parts of 1,4- cyclohexane dimethanols, 20 parts of trimethylolpropanes, 600 parts of adipic acids and 2.5 part three are taken
Sad normal-butyl tin is added in thermocouple reaction kettle, uniform stirring and is heated to 135 DEG C in the environment of being full of nitrogen, gradually
230 DEG C are heated to, continues to and 1 part of phosphorous acid and 1 part of three sad normal-butyl tin is added after water is distilled completely, and is anti-toward thermocouple
It answers in kettle gradually plus the vacuum of 7kpa, in 230 DEG C of at a temperature of sustained response 5h, 26mgKOH/g is obtained, hydroxyl value is
4mgKOH/g, viscosity are the product of 6800mpa.s；
Step 3: taking 100 parts of n-butyl acetates to be added in thermocouple reaction kettle, uniform stirring and continuous heating, simultaneously
It is purged using nitrogen, when temperature is promoted to 130 DEG C, is added by 1 part of tert butyl peroxy benzoate and 22 parts of styrene
Mixture after sustained response 3.5h, is added 24 parts of styrene, 26 parts of benzyl propionic acid, 50 parts of methylpropionic acid methyl esters, maintains reaction
Time obtains the product that viscosity is 1800mpa.s after being 1.5h；
Step 4: will be Step 1: the mixture obtained in step 2 and step 3 is added to a thermocouple reaction kettle
In, 240 DEG C of lasting 30-60min are heated to, is added after three kinds of mixing are all melted and stirred and is separately added into 50 parts
Triglycidyl isocyanurate, 300 parts of barium sulfate, 300 parts of calcium carbonate, 3 parts of levelling agents, 3 parts of optical brighteners and with always mix
The comparable natural dye of quality carries out being sufficiently mixed stirring, is then melted and is homogenized with double screw extruder, and grinding is added after cooling
It grinds in machine, finally powder is sieved according to Particle size requirements, obtain powdery paints.
The thermocouple reaction kettle is equipped with blender, the distillation column being connected with water cooled condenser, nitrogen inlet and temperature
The thermocouple reaction kettle that degree adjuster is connected.
Powder uniformity is related with the corner coverage of powdery paints on powdery paints corner；Film after the solidification of powdery paints
Effect and powdery paints it is cold-resistant it is hot it is related, condition of cure is related with gel time.
The powdery paints for taking ordinary powder coating and the application to prepare by embodiment 1, embodiment 2 and embodiment 3 below
Carry out corner coverage, cold-resistant hot and gel time measurement experiment.
Experiment one: corner coverage experiment, corner coverage be measure coating processes and under the conditions of, providing plan view
When thickness is spent, by the ratio of the corner coating thickness of painting coupon and plane coating thickness.
(1) 2 planes and two cornerwise length of 3 rod irons applied are first measured, measurement point is away from bottom 38mm
Place, environment temperature are 23 ± 2 DEG C；
(2) hole that stick upper end is passed through with steel wire is linked into baking oven preheating, heats 30min, the powder of fluidized bed at the specified temperature
End is clean and dry, and fluidisation gas source will be removed moisture sufficiently, and powder height is at least 200mm after fluidisation；Rod iron is coated by root, i.e.,
A stick is taken out from baking oven every time, is immersed in fluidized bed powder after stopping 4-5s, with 0.5r/s in the range of being 50mm toward diameter
Speed along mandrel rotate, taken away immediately after reaching planar thickness requirement, stick into and out of sulfide powder speed be less than 0.3m/
S, to guarantee that coating is uniform；
(3) temperature and time as required makes curing of coating, is cooled to 23 ± 2 DEG C, then measure, and measures every square rod
Two planes and two cornerwise values after coating, are averaged respectively, and the value that the value after coating subtracts before coating is removed again
With 2, the coating thickness of plane coating thickness and corner is just obtained.
Experimental result: the plane coating thickness and side that powdery paints prepared by embodiment 1, embodiment 2 and embodiment 3 obtains
The ratio of the coating thickness at angle is suitable, and with the ratio of ordinary powder coating closer to 1, therefore, the powder of the application preparation
Powder is more uniform on the corner of coating.
Experiment two: cold-resistant hot experiment, it is cold-resistant it is hot for measurement powdery paints after the processing of certain hot environment immediately
It puts at low ambient temperatures, then checks the damaged condition of film.
(1) film is prepared on 3 copper plates by the standard regulation of product, and place by relevant regulations.
(2) 3 samples are placed in stable to 30min in the thermostatic drying chamber for require temperature, then take out and puts rapidly
Enter to stablize the 10min into -30 ± 2 DEG C of cryogenic box.
(3) hot 30min, cold 10min are a period, and after each cycle, the repetition period dries sample and checks that film is
The degree of the defects of no cracking, disengaging.
Experimental result: the degree of defect of powdery paints prepared by embodiment 1, embodiment 2 and embodiment 3 is suitable, and
Significantly lower than the degree of the defect of ordinary powder coating, therefore, paint film defect is easy after the powder coating solidification of the application preparation
It covers.
Experiment three: gel time measurement experiment, it is solid to crosslinking that powdery paints is melt into liquid at curing temperatures, from coating
Change, coating until cannot drawwing wire required All Time be gel time.
(1) heat block is placed on no ventilation at room temperature, heat block is warming up to predetermined temperature and stablizes it at least
10min, heat block surface temperature verify can the substance of the fusing point needed for a fritter be placed in heating plate to carry out.
(2) 0.25ml sample to be tested is moved in the pit of heat block with measurement spoon, after all samples all melt immediately
Calculator is started, melting materialss are stirred with small circumference motion mode with blender, when material starts retrogradation, what is be kept stirring
Meanwhile every 2-3s by blender by improving 10min or so in thawing object, if improve be the wire drawing to be formed become fragile so that be broken and
And when cannot be again by wire drawing in melt at filiform, then stops and record the time, this time is exactly gel time.
Experimental result: the gel time of powdery paints prepared by embodiment 1, embodiment 2 and embodiment 3 is suitable, and is lower than
The gel time of ordinary powder coating, therefore, condition of cure required for the powdery paints of the application preparation are lower.
Advantageous effect of the invention is: the powdery paints and preparation method pass through the neopentyl glycol of setting, isophthalic acid and three
Sad normal-butyl tin prepares amorphous polyester, by setting Isosorbide-5-Nitrae-cyclohexane dimethanol, trimethylolpropane, adipic acid, three pungent
The sad normal-butyl tin of sour normal-butyl tin, phosphorous acid and three prepares semicrystalline polyester, by the way that n-butyl acetate, t-butyl peroxy is arranged
Change benzoic ether and styrene, styrene, benzyl propionic acid and methylpropionic acid methyl esters prepare acrylic copolymer, nothing therein is fixed
Shape polyester has polar group, and powder utilization is higher, problem that can be inhomogenous with powder on effective solution corner；Therein half
The metal adhesion of crystalline polyester is strong, and condition of cure requirement is low, can effectively reduce condition of cure；Acrylic acid copolymer therein
Object dissolves under spraying temperature, freezing film when cooling, need to only heat fusing, levelling, cooling or extraction freezing film, solution
The problem of paint film defect is difficult to conceal after certainly solidifying；And the preparation of amorphous polyester, the preparation of semicrystalline polyester and acrylic acid
The preparation of copolymer is individually being equipped with blender, the distillation column being connected with water cooled condenser, nitrogen inlet and temperature tune
It is carried out in the thermocouple reaction kettle that section device is connected, for nitrogen as protective gas, polymerization reaction is mutually indepedent in preparation process, temperature
Degree is controllable, interference-free and free from the influence of the external environment, similarly in the preparation of amorphous polyester, half in last mixing
The preparation of crystalline polyester and the preparation of acrylic copolymer are carried out in individual be equipped in blender, entire process flow institute
The instrument needed is few, and less input, and links independently carry out, and saves the time, improves preparation efficiency.
Obviously, various changes and modifications can be made to the invention without departing from essence of the invention by those skilled in the art
Mind and range.In this way, if these modifications and changes of the present invention belongs to the range of the claims in the present invention and its equivalent technologies
Within, then the present invention is also intended to include these modifications and variations.
Claims (8)
1. a kind of powdery paints, it is characterised in that: it is prepared from the following raw materials in parts by weight: 400-500 parts of neopentyl glycol,
700-800 parts of phthalic acid, three sad 6 parts of normal-butyl tin, 500-600 parts of 1,4- cyclohexane dimethanol, trimethylolpropane 10-20
Part, 500-600 parts of adipic acid, 1 part of phosphorous acid, 100 parts of n-butyl acetate, 1 part of tert butyl peroxy benzoate, styrene 24
Part, 26 parts of benzyl propionic acid, 50 parts of methylpropionic acid methyl esters.
2. a kind of powdery paints as described in claim 1, it is characterised in that: it is pungent that described three sad 6 parts of tin of normal-butyls are divided into three
2.5 parts of sour normal-butyl tin, 2.5 parts of three sad normal-butyl tin and three sad 1 part of tin of normal-butyls.
3. a kind of powdery paints as described in claim 1, it is characterised in that: the powdery paints further includes that three glycidyl are different
40-50 parts of cyanurate.
4. a kind of powdery paints as described in claim 1, it is characterised in that: the powdery paints further includes average grain diameter 20-
200-300 parts of calcium carbonate of 200-300 parts and average grain diameter 20-30 microns of 30 microns of barium sulfate.
5. a kind of powdery paints as described in claim 1, it is characterised in that: the powdery paints further includes 2-3 parts of levelling agent
With 1-3 parts of optical brightener.
6. a kind of powdery paints as described in claim 1, it is characterised in that: the powdery paints is also wrapped by cinnabar, laterite, hero
One of Huang, peacock green, powdered whiting, wollastonite, blanc fixe, talcum powder, mica powder and kaolin or a variety of mixing
20-30 microns of average grain diameter of natural dye.
7. a kind of preparation method of powdery paints, it is characterised in that: specifically includes the following steps:
Step 1: taking 450 parts of neopentyl glycols to be added in thermocouple reaction kettle, be full of nitrogen in the environment of uniform stirring and add
Heat adds 750 parts of isophthalic acids and 2.5 part of three sad normal-butyl tin, is progressively heated at 240 DEG C to 135 DEG C, from 190 DEG C, water
It is distilled out from reactor, keeps 240 DEG C of reaction 3h, the product acid value finally obtained is 38mgKOH/g, hydroxyl value 4mgKOH/
G, viscosity are the product of 2200mpa.s；
Step 2: 550 parts of 1,4- cyclohexane dimethanols, 15 parts of trimethylolpropanes, 550 parts of adipic acids and 2.5 part of three octanoic acid are taken
Normal-butyl tin is added in thermocouple reaction kettle, uniform stirring and is heated to 135 DEG C in the environment of being full of nitrogen, is gradually heated up
To 230 DEG C, continues to and 1 part of phosphorous acid and 1 part of three sad normal-butyl tin, and past thermocouple reaction kettle is added after water is distilled completely
In gradually plus the vacuum of 7kpa, in 230 DEG C of at a temperature of sustained response 5h, obtain 26mgKOH/g, hydroxyl value 4mgKOH/g,
Viscosity is the product of 6800mpa.s；
Step 3: taking 100 parts of n-butyl acetates to be added in thermocouple reaction kettle, and uniform stirring and continuous heating utilize simultaneously
The mixing by 1 part of tert butyl peroxy benzoate and 22 parts of styrene is added when temperature is promoted to 130 DEG C in nitrogen purging
Object after sustained response 3.5h, is added 24 parts of styrene, 26 parts of benzyl propionic acid, 50 parts of methylpropionic acid methyl esters, maintains the reaction time
To obtain the product that viscosity is 1800mpa.s after 1.5h；
Step 4: by Step 1: the mixture obtained in step 2 and step 3 is added in a thermocouple reaction kettle, add
Heat is added after three kinds of mixing are all melted and stirred to 240 DEG C of lasting 30-60min and is separately added into 45 parts of tricyclics
Oxygen propyl group chlorinated isocyanurates, 250 parts of barium sulfate, 250 parts of calcium carbonate, 2.5 parts of levelling agents, 1.5 parts of optical brighteners and with always mix
The comparable natural dye of quality carries out being sufficiently mixed stirring, is then melted and is homogenized with double screw extruder, and grinding is added after cooling
It grinds in machine, finally powder is sieved according to Particle size requirements, obtain powdery paints.
8. a kind of preparation method of powdery paints as claimed in claim 7, it is characterised in that: the thermocouple reaction kettle is dress
The thermocouple reaction kettle for thering is blender, the distillation column being connected with water cooled condenser, nitrogen inlet and thermoregulator to be connected.
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| CN201910580817.3A CN110330870A (en) | 2019-06-29 | 2019-06-29 | A kind of powdery paints and preparation method |
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| CN201910580817.3A CN110330870A (en) | 2019-06-29 | 2019-06-29 | A kind of powdery paints and preparation method |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111978832A (en) * | 2020-09-01 | 2020-11-24 | 常州崇高纳米材料有限公司 | Antibacterial and antiviral powder coating and preparation method thereof |
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| CN1148070A (en) * | 1995-07-12 | 1997-04-23 | 埃姆斯·英芬塔股份有限公司 | Thermosetting powder coating systems |
| DE19548491A1 (en) * | 1995-12-22 | 1997-06-26 | Inventa Ag | Thermosetting powder coating composition, for electrostatic and fluidised bed coating |
| CN1156161A (en) * | 1995-12-01 | 1997-08-06 | 埃姆斯-英维塔公司 | Thermosetting powder coating and its preparing method |
| CA2400576A1 (en) * | 2000-12-21 | 2002-06-27 | Ucb, S.A. | Powdered thermosetting composition for coatings |
| CN1404516A (en) * | 2000-12-21 | 2003-03-19 | Ucb公司 | Powdered thermosetting composition for coatings |
| CN102942837A (en) * | 2012-11-15 | 2013-02-27 | 山东海冠化工科技有限公司 | Polyester resin for one-step method low light powder paint and preparation method of polyester resin |
| CN103145962A (en) * | 2013-03-07 | 2013-06-12 | 芜湖艾力特新材料科技有限公司 | Low-temperature fast-curing energy-saving type polyester resin |
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2019
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1148070A (en) * | 1995-07-12 | 1997-04-23 | 埃姆斯·英芬塔股份有限公司 | Thermosetting powder coating systems |
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| DE19548491A1 (en) * | 1995-12-22 | 1997-06-26 | Inventa Ag | Thermosetting powder coating composition, for electrostatic and fluidised bed coating |
| CA2400576A1 (en) * | 2000-12-21 | 2002-06-27 | Ucb, S.A. | Powdered thermosetting composition for coatings |
| CN1404516A (en) * | 2000-12-21 | 2003-03-19 | Ucb公司 | Powdered thermosetting composition for coatings |
| CN102942837A (en) * | 2012-11-15 | 2013-02-27 | 山东海冠化工科技有限公司 | Polyester resin for one-step method low light powder paint and preparation method of polyester resin |
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| CN111978832A (en) * | 2020-09-01 | 2020-11-24 | 常州崇高纳米材料有限公司 | Antibacterial and antiviral powder coating and preparation method thereof |
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