CN112048236A - Extinction type thermal transfer powder coating and preparation method and application thereof - Google Patents
Extinction type thermal transfer powder coating and preparation method and application thereof Download PDFInfo
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- CN112048236A CN112048236A CN202010942611.3A CN202010942611A CN112048236A CN 112048236 A CN112048236 A CN 112048236A CN 202010942611 A CN202010942611 A CN 202010942611A CN 112048236 A CN112048236 A CN 112048236A
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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
- C09D167/06—Unsaturated polyesters having carbon-to-carbon unsaturation
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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
- C08G63/52—Polycarboxylic acids or polyhydroxy compounds in which at least one of the two components contains aliphatic unsaturation
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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
- C08G63/66—Polyesters containing oxygen in the form of ether groups
- C08G63/668—Polyesters containing oxygen in the form of ether groups derived from polycarboxylic acids and polyhydroxy compounds
- C08G63/676—Polyesters containing oxygen in the form of ether groups derived from polycarboxylic acids and polyhydroxy compounds in which at least one of the two components contains aliphatic unsaturation
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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
- C08G63/68—Polyesters containing atoms other than carbon, hydrogen and oxygen
- C08G63/685—Polyesters containing atoms other than carbon, hydrogen and oxygen containing nitrogen
- C08G63/6854—Polyesters containing atoms other than carbon, hydrogen and oxygen containing nitrogen derived from polycarboxylic acids and polyhydroxy compounds
- C08G63/6858—Polycarboxylic acids and polyhydroxy compounds in which at least one of the two components contains aliphatic unsaturation
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/03—Powdery paints
- C09D5/033—Powdery paints characterised by the additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
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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
- 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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Abstract
The invention relates to a delustering type thermal transfer powder coating and a preparation method and application thereof. A delustering type thermal transfer powder coating is characterized by comprising a component A and a component B, wherein the mass ratio of the component A to the component B is 1 (0.5-2); the component A comprises the following raw materials in parts by weight: 450-480 parts of polyester resin A with an acid value of 45-57 mgKOH/g, 30-40 parts of curing agent, 5-10 parts of flatting agent, 450-500 parts of pigment and filler and 5-10 parts of auxiliary agent; the component B comprises the following raw materials in parts by weight: 470-500 parts of polyester resin B with an acid value of 15-25 mgKOH/g, 10-20 parts of curing agent, 5-10 parts of flatting agent, 450-500 parts of pigment and filler and 5-10 parts of auxiliary agent. The extinction type thermal transfer powder coating provided by the invention is a two-component powder coating, wherein the component A and the component B respectively comprise polyester resins with different acid values, and the two polyester resins have different gel times in the curing process, so that the extinction type thermal transfer powder coating has an excellent extinction effect.
Description
Technical Field
The invention relates to the field of powder coatings, in particular to a delustering type thermal transfer powder coating and a preparation method and application thereof.
Background
In recent years, with the development of national economy and the national emphasis on environmental protection, powder coatings have met with great development opportunities. As an important branch of the thermal transfer powder coating, the thermal transfer powder coating gradually covers the furniture industry deeply. Most household products have medium and low light effects, and are mainly popularized and applied by furniture manufacturers due to unique advantages and soft wood grain texture. The mid-light transfer printing powder coating is mostly prepared by a method of adding a flatting agent; the low light transfer printing powder coating adopts polyester/TGIC (triglycidyl isocyanurate), a delustering agent system and a polyester two-component blending delustering system besides an expensive polyurethane delustering system, is widely applied to heat transfer printing at the civilian price and beautiful and diversified appearances, and is developed relatively mature at present.
As the curing agent TGIC in the powder coating has toxicity and environmental protection problems in the synthesis, post-treatment and powder coating production and construction, the curing agent TGIC is determined as a highly toxic product in Europe and makes a limited decision. TGIC is also listed in the rejected product catalog in 2010 by the Ministry of industry in China, so that the selection of a beta-hydroxyalkylamide (HAA for short) system for powder coating is a trend. However, the use of HAA systems in powder coatings is subject to problems such as sticking of the paper after transfer, unclear lines of the transferred pattern, and high gloss of the product.
Disclosure of Invention
The invention provides a delustering type thermal transfer powder coating and a preparation method and application thereof to overcome the defects in the prior art.
In order to achieve the above purpose, the invention is realized by the following technical scheme:
a delustering type thermal transfer powder coating is characterized by comprising a component A and a component B, wherein the mass ratio of the component A to the component B is 1 (0.5-2);
the component A comprises the following raw materials in parts by weight: 450-480 parts of polyester resin A with an acid value of 45-57 mgKOH/g, 30-40 parts of curing agent, 5-10 parts of flatting agent, 450-500 parts of pigment and filler and 5-10 parts of auxiliary agent;
the component B comprises the following raw materials in parts by weight: 470-500 parts of polyester resin B with an acid value of 15-25 mgKOH/g, 10-20 parts of curing agent, 5-10 parts of flatting agent, 450-500 parts of pigment and filler and 5-10 parts of auxiliary agent.
According to one embodiment of the invention, the polyester resin A with the acid value of 45-57 mgKOH/g has the viscosity of 5000-10500 mPa.s at 200 ℃ and the gelling time of 40-120 s at 180 ℃; the polyester resin B with the acid value of 15-25 mgKOH/g has the viscosity of 5000-10500 mPa & s at 200 ℃ and the gelling time of 400-700 s at 180 ℃.
According to one embodiment of the invention, the polyester resin A with the acid value of 45-57 mgKOH/g is prepared by polymerizing the following raw material components in parts by weight: 100-200 parts of terephthalic acid, 100-400 parts of isophthalic acid, 50-100 parts of adipic acid, 50-100 parts of fumaric acid, 100-500 parts of dihydric alcohol, 20-200 parts of a cross-linking agent, 0.5-4 parts of a catalyst and 0.5-4 parts of an antioxidant.
According to one embodiment of the invention, the polyester resin B with the acid value of 15-25 mgKOH/g is prepared by polymerizing the following raw material components in parts by weight: 20-200 parts of terephthalic acid, 40-400 parts of isophthalic acid, 10-100 parts of adipic acid, 10-100 parts of fumaric acid, 50-100 parts of 1, 4-cyclohexanedicarboxylic acid, 100-500 parts of dihydric alcohol, 20-200 parts of a crosslinking agent, 0.5-4 parts of a catalyst and 0.5-4 parts of an antioxidant.
According to an embodiment of the present invention, the diol includes one or more of neopentyl glycol, 1, 4-butanediol, 1, 4-cyclohexanedimethanol, diethylene glycol, trimethylpentanediol, 2-methyl-1, 3-propanediol; the cross-linking agent comprises one or more than two of trimethylolpropane, trimethylolethane, tris (hydroxyethyl) isocyanurate and pentaerythritol; the catalyst comprises monobutyltin oxide and/or dibutyltin oxide; the antioxidant comprises one or more than two of antioxidant 1001, antioxidant 1010, antioxidant 1076, antioxidant 300 and antioxidant 168.
According to one embodiment of the invention, the curing agent is a β -hydroxyalkylamide.
According to one embodiment of the invention, the leveling agent is selected from BLP503, the pigment filler comprises titanium dioxide, barium sulfate and/or barite, and the auxiliary agent is selected from benzoin.
The preparation method of the extinction type thermal transfer powder coating is characterized by comprising the following steps:
preparing polyester resin A and polyester resin B; and then uniformly mixing the polyester resin A and the polyester resin B with a curing agent, a flatting agent, a pigment filler and an auxiliary agent according to a ratio, then performing melt extrusion, grinding and screening to obtain a component A and a component B, and finally mixing the component A and the component B according to a mass ratio of 1 (0.5-2).
According to one embodiment of the present invention, the preparation method of the polyester resin a comprises the steps of:
(1) placing the dihydric alcohol and the cross-linking agent in a formula amount into a reaction kettle, heating to 110-130 ℃ to completely melt the added dihydric alcohol and the cross-linking agent, continuously adding terephthalic acid, adipic acid, fumaric acid and a catalyst, heating to 240-250 ℃ under the protection of nitrogen to react for at least 3 hours until the resin is transparent, and testing the acid value of the resin;
(2) cooling to 220 ℃, adding isophthalic acid, continuing to react for 2-3 hours until the resin is clear and transparent, and testing the acid value of the resin;
(3) and (3) continuously reacting for 2-4 h under a vacuum condition until the acid value is 45-57 mgKOH/g, adding an antioxidant, uniformly stirring, cooling to 200 ℃, and discharging to obtain the polyester resin A.
According to one embodiment of the present invention, the preparation method of the polyester resin B comprises the steps of:
(1) placing the dihydric alcohol and the cross-linking agent in a formula amount into a reaction kettle, heating to 110-130 ℃ to completely melt the added dihydric alcohol and the cross-linking agent, continuously adding terephthalic acid, adipic acid, fumaric acid and a catalyst, heating to 240-250 ℃ under the protection of nitrogen to react for at least 3 hours until the resin is transparent, and testing the acid value of the resin;
(2) cooling to 220 ℃, adding isophthalic acid, continuing to react for 2-3 hours until the resin is clear and transparent, and testing the acid value of the resin;
(3) continuously reacting for 2-4 h under the vacuum condition until the acid value is 15-25 mgKOH/g, adding an antioxidant,
and cooling to 200 ℃ after uniform stirring, and discharging to obtain the polyester resin B.
According to an embodiment of the present invention, the diol includes one or more of neopentyl glycol, 1, 4-butanediol, 1, 4-cyclohexanedimethanol, diethylene glycol, trimethylpentanediol, 2-methyl-1, 3-propanediol; the cross-linking agent comprises one or more than two of trimethylolpropane, trimethylolethane, tris (hydroxyethyl) isocyanurate and pentaerythritol; the catalyst is monobutyl tin oxide and/or dibutyl tin oxide; the antioxidant comprises one or more than two of antioxidant 1001, antioxidant 1010, antioxidant 1076, antioxidant 300 and antioxidant 168.
According to one embodiment of the invention, the curing agent is a β -hydroxyalkylamide; the leveling agent is selected from BLP503, the pigment filler comprises titanium dioxide, barium sulfate and/or barite, and the auxiliary agent is selected from benzoin.
The application of the extinction type thermal transfer powder coating or the extinction type thermal transfer powder coating obtained by the preparation method is characterized in that the extinction type thermal transfer powder coating is electrostatically sprayed on a metal plate subjected to oil and scale removal, then the metal plate is placed in a constant-temperature oven at 200 ℃ to be cured for more than 10min to obtain the extinction type thermal transfer powder coating, and finally, a transfer template is obtained through thermal transfer.
The extinction type thermal transfer powder coating provided by the invention is a two-component powder coating, wherein the component A and the component B respectively comprise polyester resins with different acid values, and the two polyester resins have different gel times in the curing process, so that the extinction type thermal transfer powder coating has an excellent extinction effect. Moreover, the extinction type powder coating adopts a polyester/HAA curing system, so that the problems of toxic pollution caused by using curing agent TGIC and paper sticking and difficult paper tearing caused by using curing agent HAA in the prior art are solved; the obtained final product is more environment-friendly. The invention also provides a preparation method of the extinction type thermal transfer printing powder coating, the pattern obtained by thermal transfer printing of the extinction type powder coating is clear, paper is easy to tear, no paper is stuck, the extinction effect of a product after thermal transfer printing is good, and the glossiness (60 ℃) is 10% -30%.
Detailed Description
The present invention will be described in detail with reference to examples.
The invention provides a delustering type thermal transfer powder coating which comprises a component A and a component B, wherein the mass ratio of the component A to the component B is 1 (0.5-2); wherein the component A comprises the following raw materials in parts by weight: 450-480 parts of polyester resin A with an acid value of 45-57 mgKOH/g, 30-40 parts of curing agent, 5-10 parts of flatting agent, 450-500 parts of pigment and filler and 5-10 parts of auxiliary agent; the component B comprises the following raw materials in parts by weight: 470-500 parts of polyester resin B with an acid value of 15-25 mgKOH/g, 10-20 parts of curing agent, 5-10 parts of flatting agent, 450-500 parts of pigment and filler and 5-10 parts of auxiliary agent. The thermal transfer powder coating is a two-component powder coating, and the gelation time of the component A and the component B in the curing process can be different, so that the thermal transfer powder coating has an excellent extinction effect.
Wherein the polyester resin A with the acid value of 45-57 mgKOH/g has the viscosity of 5000-10500 mPa & s at 200 ℃ and the gelling time of 40-120 s at 180 ℃; the polyester resin B having an acid value of 15 to 25mgKOH/g has a viscosity of 5000 to 10500 mPas at 200 ℃ and a gel time of 400 to 700s at 180 ℃. Due to the fact that the component A and the component B comprise the polyester resin A and the polyester resin B with different acid values, the difference between fast curing and slow curing of the two components is caused, and therefore the surface coated by the powder coating forms a micro rough surface which plays a role of reflecting light.
The polyester resin A is prepared by polymerizing the following raw material components in parts by weight: 100-200 parts of terephthalic acid, 100-400 parts of isophthalic acid, 50-100 parts of adipic acid, 50-100 parts of fumaric acid, 100-500 parts of dihydric alcohol, 20-200 parts of a cross-linking agent, 0.5-4 parts of a catalyst and 0.5-4 parts of an antioxidant.
The polyester resin B is prepared by polymerizing the following raw material components in parts by weight: 20-200 parts of terephthalic acid, 40-400 parts of isophthalic acid, 10-100 parts of adipic acid, 10-100 parts of fumaric acid, 50-100 parts of 1, 4-cyclohexanedicarboxylic acid, 100-500 parts of dihydric alcohol, 20-200 parts of a crosslinking agent, 0.5-4 parts of a catalyst and 0.5-4 parts of an antioxidant.
Wherein the dihydric alcohol comprises one or more of neopentyl glycol, 1, 4-butanediol, 1, 4-cyclohexanedimethanol, diethylene glycol, trimethylpentanediol and 2-methyl-1, 3-propanediol; the cross-linking agent comprises one or more than two of trimethylolpropane, trimethylolethane, tris (hydroxyethyl) isocyanurate and pentaerythritol; the catalyst comprises monobutyl tin oxide and/or dibutyl tin oxide; the antioxidant comprises one or more of antioxidant 1001, antioxidant 1010, antioxidant 1076, antioxidant 300 and antioxidant 168.
In the present invention, the curing agent is a β -hydroxyalkylamide. The powder coating of the invention belongs to a polyester/HAA curing system, has clear patterns after thermal transfer printing, is simple and easy to tear paper, does not stick paper, and overcomes the common problems of the HAA curing agent when used in the powder coating.
The leveling agent in the powder coating is selected from BLP503, the pigment and filler comprise titanium dioxide, barium sulfate and/or barite, and the auxiliary agent is selected from benzoin.
The matte thermal transfer powder coating obtained in the invention adopts a polyester/HAA curing system, and the inventor of the invention finds that the component A and the component B of the powder coating are respectively prepared from the polyester resin A with the acid value of 45-57 mgKOH/g and the polyester resin B with the acid value of 15-25 mgKOH/g, and then the component A and the component B are mixed to obtain the powder coating with excellent matte effect. The difference between the acid values of the polyester resins causes the two to form a relatively fast component and a relatively slow component during the curing process, respectively, so that the gel time is different, and a microscopic rough surface is formed after the polyester resins are melted and cured, and the rough surface diffusely reflects light, thereby playing a role in reducing the glossiness. The extinction type thermal transfer powder coating has an excellent extinction effect in application.
The invention also provides a preparation method of the extinction type thermal transfer powder coating, which comprises the following steps:
preparing polyester resin A and polyester resin B; and then uniformly mixing the polyester resin A and the polyester resin B with a curing agent, a flatting agent, a pigment filler and an auxiliary agent according to a ratio, performing melt extrusion, grinding and screening to obtain a component A and a component B, and finally mixing the component A and the component B according to a mass ratio of 1 (0.5-2).
The preparation method of the polyester resin A comprises the following steps:
(1) placing the dihydric alcohol and the cross-linking agent in a formula amount into a reaction kettle, heating to 110-130 ℃ to completely melt the added dihydric alcohol and the cross-linking agent, continuously adding terephthalic acid, adipic acid, fumaric acid and a catalyst, heating to 240-250 ℃ under the protection of nitrogen to react for at least 3 hours until the resin is transparent, and testing the acid value of the resin;
(2) cooling to 220 ℃, adding isophthalic acid, continuing to react for 2-3 hours until the resin is clear and transparent, and testing the acid value of the resin;
(3) and (3) continuously reacting for 2-4 h under a vacuum condition until the acid value is 45-57 mgKOH/g, adding an antioxidant, uniformly stirring, cooling to 200 ℃, discharging, and obtaining the polyester resin A with the acid value of 45-57 mgKOH/g.
The preparation method of the polyester resin B comprises the following steps:
(1) placing the dihydric alcohol and the cross-linking agent in a formula amount into a reaction kettle, heating to 110-130 ℃ to completely melt the added dihydric alcohol and the cross-linking agent, continuously adding terephthalic acid, adipic acid, fumaric acid and a catalyst, heating to 240-250 ℃ under the protection of nitrogen to react for at least 3 hours until the resin is transparent, and testing the acid value of the resin;
(2) cooling to 220 ℃, adding isophthalic acid, continuing to react for 2-3 hours until the resin is clear and transparent, and testing the acid value of the resin;
(3) and (3) continuously reacting for 2-4 h under a vacuum condition until the acid value is 15-25 mgKOH/g, adding an antioxidant, uniformly stirring, cooling to 200 ℃, and discharging to obtain the polyester resin B.
In the preparation method of the polyester resin A and the polyester resin B, the dihydric alcohol comprises one or more than two of neopentyl glycol, 1, 4-butanediol, 1, 4-cyclohexanedimethanol, diethylene glycol, trimethylpentanediol and 2-methyl-1, 3-propanediol; the cross-linking agent comprises one or more than two of trimethylolpropane, trimethylolethane, tris (hydroxyethyl) isocyanurate and pentaerythritol; the catalyst is monobutyl tin oxide and/or dibutyl tin oxide; the antioxidant comprises one or more of antioxidant 1001, antioxidant 1010, antioxidant 1076, antioxidant 300 and antioxidant 168.
In the preparation method of the extinction type thermal transfer powder coating, the curing agent is beta-hydroxyalkylamide; the leveling agent is selected from BLP503, the pigment and filler comprises titanium dioxide, barium sulfate and/or barite, and the auxiliary agent is selected from benzoin.
According to the mixture ratio: uniformly mixing the polyester resin A or the polyester resin B with a curing agent, a flatting agent, a pigment filler and an auxiliary agent; and then extruding, tabletting, cooling, crushing and sieving by a double-screw extruder to finally prepare the extinction type thermal transfer powder coating.
The invention also provides application of the extinction type thermal transfer powder coating or the extinction type thermal transfer powder coating obtained by the preparation method, the extinction type thermal transfer powder coating is electrostatically sprayed on a metal plate which is degreased and descaled, then the metal plate is placed in a constant temperature oven at 200 ℃ to be solidified for more than 10min to obtain the extinction type thermal transfer powder coating, and finally a transfer template is obtained through thermal transfer printing, wherein the temperature of the thermal transfer printing is 200 ℃ and the time is 180 s.
The extinction type thermal transfer powder coating is subjected to thermal transfer printing to obtain clear patterns, the paper is easy to tear, the paper is not stuck, the extinction effect of a product subjected to thermal transfer printing is good, and the glossiness (60 ℃) is 10% -30%.
Example 1
Preparation of component A: putting 25 parts of neopentyl glycol, 25 parts of 1, 4-cyclohexanedimethanol, 50 parts of diethylene glycol and 20 parts of trimethylolpropane into a first synthesis reaction kettle, opening a jacket heat conduction oil valve, and heating to 110 ℃ until the materials are completely molten; adding 100 parts of terephthalic acid, 50 parts of adipic acid, 50 parts of fumaric acid and 0.5 part of monobutyl tin oxide, covering a kettle cover, opening nitrogen protection, heating to 240 ℃ for esterification reaction, keeping the resin transparent, and sampling to measure the acid value to be 32 mgKOH/g; the temperature is reduced to 220 ℃, 100 parts of isophthalic acid is added, the reaction is continued for 2 hours, and the sampling acid value is measured to be 50 mgKOH/g. Reacting under vacuum condition with pressure of-0.098 MPa for 2 hr, sampling to obtain a measured acid value of 45mgKOH/g, viscosity of 5000 mPas at 200 deg.C, and gelling time of 40s at 180 deg.C; at this time, 0.5 part of antioxidant 1001 is added, stirred uniformly and cooled to 200 ℃, and then discharged, so as to obtain the polyester resin A with the acid value of 45 mgKOH/g. The component A is prepared by uniformly mixing 450 parts of the polyester resin A, 30 parts of beta-hydroxyalkylamide, 5 parts of a flatting agent BLP50 (selected from Ningbo south sea chemical Co., Ltd.), 450 parts of titanium dioxide and 5 parts of benzoin, and then carrying out melt extrusion, grinding and screening.
Preparation of component B: adding 25 parts of 1, 4-butanediol, 25 parts of 1, 4-cyclohexanedimethanol, 50 parts of diethylene glycol and 20 parts of trimethylolpropane into a second synthesis reaction kettle, opening a jacket heat-conducting oil valve, and heating to 110 ℃ until the materials are completely molten; adding 20 parts of terephthalic acid, 10 parts of adipic acid, 10 parts of fumaric acid, 0.5 part of monobutyl tin oxide and 50 parts of 1, 4-cyclohexanedicarboxylic acid, covering a kettle cover, opening nitrogen protection, heating to 240 ℃ for esterification reaction, keeping the resin transparent, and sampling to measure the acid value to be 10 mgKOH/g; the temperature is reduced to 220 ℃, 40 parts of isophthalic acid is added, the reaction is continued for 2 hours, and the sampling acid value is measured to be 20 mgKOH/g. Reacting under vacuum condition with pressure of-0.098 MPa for 2 hr, sampling to obtain a measured acid value of 15mgKOH/g, viscosity of 5000 mPas at 200 deg.C, and gelling time of 400s at 180 deg.C; at this time, 0.5 part of antioxidant 1001 is added, stirred uniformly and cooled to 200 ℃, and then discharged, so as to obtain the polyester resin B with the acid value of 15 mgKOH/g. 470 parts of the polyester resin B, 10 parts of beta-hydroxyalkylamide, 5 parts of a flatting agent BLP50 (selected from Ningbo south sea chemical Co., Ltd.), 450 parts of titanium dioxide and 5 parts of benzoin are uniformly mixed, and then the component B is prepared by melt extrusion, grinding and screening.
Uniformly mixing the component A and the component B in a mass ratio of 1:0.5 to obtain the extinction type thermal transfer powder coating 1. The extinction type thermal transfer printing powder coating 1 is electrostatically sprayed on an iron plate which is degreased and descaled, and then is put into a constant temperature oven at 200 ℃ for curing for 10min to obtain an extinction type thermal transfer printing powder coating; and (3) performing heat source transfer printing for 180s at 200 ℃ by using a transfer printing machine, and finally cooling and tearing off transfer printing paper to obtain the thermal transfer printing sample plate 1.
Example 2
Preparation of component A: putting 100 parts of neopentyl glycol, 45 parts of 1, 4-cyclohexanedimethanol, 55 parts of trimethylpentanediol, 30 parts of trimethylolpropane and 50 parts of trimethylolethane into a first synthesis reaction kettle, opening a jacket heat conduction oil valve, and heating to 115 ℃ until all materials are molten; adding 130 parts of terephthalic acid, 70 parts of adipic acid, 70 parts of fumaric acid and 2 parts of monobutyl tin oxide, covering a kettle cover, starting nitrogen protection, gradually heating to 245 ℃ for esterification reaction, keeping the resin transparent, and sampling to measure the acid value to be 37 mgKOH/g; the temperature is reduced to 220 ℃, 200 parts of isophthalic acid is added, the reaction is continued for 2.5 hours, and the sampling acid value is measured to be 52 mgKOH/g. Reacting under vacuum condition with pressure of-0.098 MPa for 2.5 hr, sampling to obtain a measured acid value of 48mgKOH/g, viscosity of 8000 mPas at 200 deg.C, and gelling time of 70s at 180 deg.C; at this time, 1 part of antioxidant 168 is added, stirred uniformly and cooled to 200 ℃, and then discharged, thus obtaining the polyester resin A with the acid value of 48 mgKOH/g. 465 parts of the polyester resin A, 31 parts of beta-hydroxyalkylamide, 6 parts of a flatting agent BLP50 (selected from Ningbo south sea chemical Co., Ltd.), 470 parts of barium sulfate and 7 parts of benzoin are uniformly mixed, and then the component A is prepared by melt extrusion, grinding and screening.
Preparation of component B: putting 75 parts of 1, 4-butanediol, 25 parts of 1, 4-cyclohexanedimethanol, 50 parts of diethylene glycol, 30 parts of trimethylolpropane and 60 parts of trimethylolethane into a second synthesis reaction kettle, opening a jacket heat conduction oil valve, heating to 115 ℃, and completely melting the materials; adding 100 parts of terephthalic acid, 50 parts of adipic acid, 30 parts of fumaric acid, 1.5 parts of monobutyl tin oxide and 70 parts of 1, 4-cyclohexanedicarboxylic acid, covering a kettle cover, opening nitrogen protection, heating to 245 ℃ for esterification reaction, keeping the resin transparent, and sampling to measure the acid value to be 13 mgKOH/g; the temperature is reduced to 220 ℃, 100 parts of isophthalic acid is added, the reaction is continued for 2.5 hours, and the sampling acid value is measured to be 22 mgKOH/g. Reacting under vacuum condition with pressure of-0.098 MPa for 2.5 hr, sampling to measure acid value of 20mgKOH/g, viscosity of 8000 mPas at 200 deg.C, and gelling time of 500s at 180 deg.C; then adding 1 part of antioxidant 1001 and 0.5 part of antioxidant 1010, uniformly stirring, cooling to 200 ℃, discharging, and obtaining the polyester resin B with the acid value of 20 mgKOH/g. 485 parts of the polyester resin B, 13 parts of beta-hydroxyalkylamide, 6 parts of a flatting agent BLP50 (selected from Ningbo south sea chemical Co., Ltd.), 250 parts of titanium dioxide, 225 parts of barium sulfate and 7 parts of benzoin are uniformly mixed, and then the mixture is subjected to melt extrusion, grinding and screening to obtain a component B.
Uniformly mixing the component A and the component B in a mass ratio of 1:1 to obtain the extinction type thermal transfer powder coating 2. The extinction type thermal transfer printing powder coating 2 is electrostatically sprayed on an iron plate which is degreased and descaled, and then is put into a constant temperature oven at 200 ℃ for curing for 12min to obtain an extinction type thermal transfer printing powder coating; and (3) performing heat transfer printing for 180s at 200 ℃ by a transfer printing machine, and finally cooling and tearing off transfer printing paper to obtain the thermal transfer printing sample plate 2.
Example 3
Preparation of component A: adding 180 parts of neopentyl glycol, 100 parts of trimethylpentane diol, 20 parts of 2-methyl-1, 3-propanediol, 80 parts of trimethylolpropane and 70 parts of tris (hydroxyethyl) isocyanurate into a first synthesis reaction kettle, opening a jacket heat-conducting oil valve, and heating to 120 ℃ until the materials are completely molten; 150 parts of terephthalic acid, 80 parts of adipic acid, 75 parts of fumaric acid, 2 parts of monobutyl tin oxide and 1 part of dibutyl tin oxide are added, a kettle cover is covered, nitrogen protection is opened, the temperature is gradually increased to 245 ℃ for esterification reaction, the resin is maintained to be transparent, and the sampling acid value is 50 mgKOH/g; the temperature is reduced to 220 ℃, 300 parts of isophthalic acid is added, the reaction is continued for 3 hours, and the sampling acid value is measured to be 60 mgKOH/g. Reacting under vacuum condition with pressure of-0.098 MPa for 3 hr, sampling to obtain a sample with acid value of 52mgKOH/g, viscosity of 10000 mPa.s at 200 deg.C, and gelling time of 100s at 180 deg.C; then, 1.5 parts of antioxidant 1010 and 1.5 parts of antioxidant 1076 are added, stirred uniformly and cooled to 200 ℃, and then the polyester resin A with the acid value of 52mgKOH/g is obtained. 475 parts of the polyester resin A, 39 parts of beta-hydroxyalkylamide, 9 parts of a flatting agent BLP50 (selected from Ningbo south sea chemical Co., Ltd.), 480 parts of barite and 9 parts of benzoin are uniformly mixed, and then the mixture is subjected to melt extrusion, grinding and screening to prepare a component A.
Preparation of component B: adding 75 parts of trimethylpentane glycol, 145 parts of 2-methyl-1, 3-propanediol, 80 parts of diethylene glycol, 80 parts of trimethylolpropane and 50 parts of pentaerythritol into a second synthesis reaction kettle, opening a jacket heat-conducting oil valve, and heating to 120 ℃ until the materials are completely melted; 150 parts of terephthalic acid, 75 parts of adipic acid, 60 parts of fumaric acid, 2.5 parts of dibutyltin oxide and 90 parts of 1, 4-cyclohexanedicarboxylic acid are added, a kettle cover is covered, nitrogen protection is opened, the temperature is raised to 245 ℃ for esterification reaction, the resin is maintained to be transparent, and the sampling acid value is 21 mgKOH/g; the temperature is reduced to 220 ℃, 300 parts of isophthalic acid is added, the reaction is continued for 3 hours, and the sampling acid value is measured to be 28 mgKOH/g. Reacting under vacuum condition with pressure of-0.098 MPa for 3 hr, sampling to measure acid value of 22mgKOH/g, viscosity of 10000 mPa.s at 200 deg.C, and gelling time of 600s at 180 deg.C; then, adding 1 part of antioxidant 300 and 2 parts of antioxidant 168, uniformly stirring, cooling to 200 ℃, discharging, and obtaining the polyester resin B with the acid value of 22 mgKOH/g. 495 parts of the polyester resin B, 18 parts of beta-hydroxyalkylamide, 9 parts of a flatting agent BLP50 (selected from Ningbo south sea chemical Co., Ltd.), 250 parts of titanium dioxide, 230 parts of barite and 9 parts of benzoin are uniformly mixed, and then the mixture is subjected to melt extrusion, grinding and screening to obtain a component B.
And uniformly mixing the component A and the component B in a mass ratio of 1:1.5 to obtain the extinction type thermal transfer powder coating 3. The extinction type thermal transfer printing powder coating 3 is electrostatically sprayed on an iron plate which is degreased and descaled, and then is put into a constant temperature oven at 200 ℃ for curing for 10min to obtain an extinction type thermal transfer printing powder coating; and (3) performing heat transfer printing for 180s at 200 ℃ by a heat source of a transfer printing machine, and finally cooling and tearing off transfer printing paper to obtain the thermal transfer printing sample plate 3.
Example 4
Preparation of component A: putting 200 parts of 1, 4-butanediol, 300 parts of 2-methyl-1, 3-propanediol and 200 parts of pentaerythritol into a first synthesis reaction kettle, opening a jacket heat conduction oil valve, and heating to 130 ℃ until the materials are completely molten; adding 200 parts of terephthalic acid, 100 parts of adipic acid, 100 parts of fumaric acid and 4 parts of dibutyltin oxide, covering a kettle cover, starting nitrogen protection, gradually heating to 250 ℃ for esterification reaction, keeping the resin transparent, and sampling to measure the acid value to be 50 mgKOH/g; the temperature is reduced to 220 ℃, 400 parts of isophthalic acid is added, the reaction is continued for 3 hours, and the sampling acid value is measured to be 60 mgKOH/g. Reacting under vacuum condition with pressure of-0.098 MPa for 4 hr, sampling to obtain a sample with acid value of 57mgKOH/g, viscosity of 10500 mPa.s at 200 deg.C, and gelation time of 120s at 180 deg.C; then, 2 parts of antioxidant 300 and 2 parts of antioxidant 168 are added, stirred uniformly and cooled to 200 ℃, and then discharged, thus obtaining the polyester resin A with the acid value of 57 mgKOH/g. 480 parts of the polyester resin A, 40 parts of beta-hydroxyalkylamide, 10 parts of a flatting agent BLP50 (selected from Ningbo south sea chemical Co., Ltd.), 200 parts of titanium dioxide, 100 parts of barium sulfate, 200 parts of barite and 10 parts of benzoin are uniformly mixed, and then the component A is prepared by melt extrusion, grinding and screening.
Preparation of component B: adding 170 parts of trimethylpentane glycol, 130 parts of neopentyl glycol, 200 parts of diethylene glycol, 80 parts of tris (hydroxyethyl) isocyanurate and 120 parts of pentaerythritol into a second synthesis reaction kettle, opening a jacket heat-conducting oil valve, and heating to 130 ℃ until the materials are completely molten; putting 200 parts of terephthalic acid, 100 parts of adipic acid, 100 parts of fumaric acid, 2 parts of monobutyl tin oxide, 2 parts of dibutyl tin oxide and 100 parts of 1, 4-cyclohexanedicarboxylic acid, covering a kettle cover, opening nitrogen protection, heating to 250 ℃ for esterification reaction, keeping the resin transparent, and sampling to measure the acid value to be 21 mgKOH/g; the temperature is reduced to 220 ℃, 400 parts of isophthalic acid is added, the reaction is continued for 3 hours, and the sampling acid value is measured to be 28 mgKOH/g. Reacting under vacuum condition with pressure of-0.098 MPa for 4 hr, sampling to measure acid value of 25mgKOH/g, viscosity of 10500 mPa.s at 200 deg.C, and gelation time of 700s at 180 deg.C; then 4 parts of antioxidant 1076 are added, the mixture is cooled to 200 ℃ after being evenly stirred, and then the mixture is discharged, thus obtaining the polyester resin B with the acid value of 25 mgKOH/g. The component B is prepared by uniformly mixing 500 parts of the polyester resin B, 20 parts of beta-hydroxyalkylamide, 10 parts of a flatting agent BLP50 (selected from Ningbo south sea chemical Co., Ltd.), 500 parts of barite and 10 parts of benzoin, and then carrying out melt extrusion, grinding and screening.
And uniformly mixing the component A and the component B in a mass ratio of 1:2 to obtain the extinction type thermal transfer powder coating 4. The extinction type thermal transfer powder coating 4 is electrostatically sprayed on an iron plate which is degreased and descaled, and then is put into a constant temperature oven at 200 ℃ for curing for 10min to obtain an extinction type thermal transfer powder coating; and (3) performing heat transfer printing for 180s at 200 ℃ by a transfer printing machine, and finally cooling and tearing off transfer printing paper to obtain the thermal transfer printing sample plate 4.
In examples 1 to 4, the acid value was measured in accordance with GB/T6743-2008, and the viscosity was measured in accordance with GB/T9751.1-2008.
The thermal transfer templates 1-4 prepared in the embodiments 1-4 of the invention are subjected to performance tests shown in the table I, wherein the gloss of the thermal transfer templates is detected according to the GB/T9754-2007 standard, the gel time is detected according to the GB/T1699-1997 standard, the impact resistance is detected according to the GB/T1732-1993 standard, the leveling property is detected according to the GB/T1750-1979 standard, the adhesion force is detected according to the GB/T9286-1988 standard, and the QUV aging is detected according to the GB/T1865-2009 standard.
Watch 1
As can be seen from the table I and the examples, the extinction type thermal transfer powder coating adopts a polyester/HAA curing system, overcomes the toxic pollution problem of curing agent TGIC in the prior art, and overcomes the problems of paper sticking and paper tearing difficulty of curing agent HAA in the prior art; the surface obtained by coating the powder coating has an excellent extinction effect, and the pattern is clear after thermal transfer printing, the paper is easy to tear, and the paper is not sticky.
The embodiments of the present invention are merely illustrative, and not restrictive, of the scope of the claims, and other substantially equivalent alternatives may occur to those skilled in the art and are within the scope of the present invention.
Claims (13)
1. A delustering type thermal transfer powder coating is characterized by comprising a component A and a component B, wherein the mass ratio of the component A to the component B is 1 (0.5-2);
the component A comprises the following raw materials in parts by weight: 450-480 parts of polyester resin A with an acid value of 45-57 mgKOH/g, 30-40 parts of curing agent, 5-10 parts of flatting agent, 450-500 parts of pigment and filler and 5-10 parts of auxiliary agent;
the component B comprises the following raw materials in parts by weight: 470-500 parts of polyester resin B with an acid value of 15-25 mgKOH/g, 10-20 parts of curing agent, 5-10 parts of flatting agent, 450-500 parts of pigment and filler and 5-10 parts of auxiliary agent.
2. A matting heat transfer powder coating according to claim 1, wherein said polyester resin A having an acid value of 45 to 57mgKOH/g has a viscosity of 5000 to 10500mPa · s at 200 ℃ and a gel time of 40 to 120s at 180 ℃; the polyester resin B with the acid value of 15-25 mgKOH/g has the viscosity of 5000-10500 mPa & s at 200 ℃ and the gelling time of 400-700 s at 180 ℃.
3. A extinction type thermal transfer powder coating according to claim 2, characterized in that the polyester resin A with the acid value of 45-57 mgKOH/g is polymerized by the following raw material components in parts by weight: 100-200 parts of terephthalic acid, 100-400 parts of isophthalic acid, 50-100 parts of adipic acid, 50-100 parts of fumaric acid, 100-500 parts of dihydric alcohol, 20-200 parts of a cross-linking agent, 0.5-4 parts of a catalyst and 0.5-4 parts of an antioxidant.
4. A extinction type thermal transfer powder coating according to claim 2, wherein the polyester resin B with the acid value of 15-25 mgKOH/g is prepared by polymerizing the following raw material components in parts by weight: 20-200 parts of terephthalic acid, 40-400 parts of isophthalic acid, 10-100 parts of adipic acid, 10-100 parts of fumaric acid, 50-100 parts of 1, 4-cyclohexanedicarboxylic acid, 100-500 parts of dihydric alcohol, 20-200 parts of a crosslinking agent, 0.5-4 parts of a catalyst and 0.5-4 parts of an antioxidant.
5. A matting type heat transfer powder coating according to claim 3 or 4, wherein said diol comprises one or more of neopentyl glycol, 1, 4-butanediol, 1, 4-cyclohexanedimethanol, diethylene glycol, trimethylpentanediol, 2-methyl-1, 3-propanediol; the cross-linking agent comprises one or more than two of trimethylolpropane, trimethylolethane, tris (hydroxyethyl) isocyanurate and pentaerythritol; the catalyst comprises monobutyltin oxide and/or dibutyltin oxide; the antioxidant comprises one or more than two of antioxidant 1001, antioxidant 1010, antioxidant 1076, antioxidant 300 and antioxidant 168.
6. A matting heat transfer powder coating according to claim 1, characterised in that said curing agent is a β -hydroxyalkylamide.
7. A matting heat transfer powder coating according to claim 1, wherein said levelling agent is selected from BLP503, said pigment fillers include titanium dioxide, barium sulfate and/or barite, and said assistant is selected from benzoin.
8. A preparation method of a extinction type thermal transfer powder coating as claimed in any one of claims 1 to 7, characterized by comprising the following steps:
preparing polyester resin A and polyester resin B; and then uniformly mixing the polyester resin A and the polyester resin B with a curing agent, a flatting agent, a pigment filler and an auxiliary agent according to a ratio, then performing melt extrusion, grinding and screening to obtain a component A and a component B, and finally mixing the component A and the component B according to a mass ratio of 1 (0.5-2).
9. A method for preparing a extinction type thermal transfer powder coating according to claim 8, wherein the method for preparing the polyester resin A comprises the following steps:
(1) placing the dihydric alcohol and the cross-linking agent in a formula amount into a reaction kettle, heating to 110-130 ℃ to completely melt the added dihydric alcohol and the cross-linking agent, continuously adding terephthalic acid, adipic acid, fumaric acid and a catalyst, heating to 240-250 ℃ under the protection of nitrogen to react for at least 3 hours until the resin is transparent, and testing the acid value of the resin;
(2) cooling to 220 ℃, adding isophthalic acid, continuing to react for 2-3 hours until the resin is clear and transparent, and testing the acid value of the resin;
(3) and (3) continuously reacting for 2-4 h under a vacuum condition until the acid value is 45-57 mgKOH/g, adding an antioxidant, uniformly stirring, cooling to 200 ℃, and discharging to obtain the polyester resin A.
10. A method for preparing a matting type thermal transfer powder coating according to claim 8, wherein said polyester resin B is prepared by a method comprising the steps of:
(1) placing the dihydric alcohol and the cross-linking agent in a formula amount into a reaction kettle, heating to 110-130 ℃ to completely melt the added dihydric alcohol and the cross-linking agent, continuously adding terephthalic acid, adipic acid, fumaric acid and a catalyst, heating to 240-250 ℃ under the protection of nitrogen to react for at least 3 hours until the resin is transparent, and testing the acid value of the resin;
(2) cooling to 220 ℃, adding isophthalic acid, continuing to react for 2-3 hours until the resin is clear and transparent, and testing the acid value of the resin;
(3) and (3) continuously reacting for 2-4 h under a vacuum condition until the acid value is 15-25 mgKOH/g, adding an antioxidant, uniformly stirring, cooling to 200 ℃, and discharging to obtain the polyester resin B.
11. A method for preparing a matting type heat transfer powder coating according to claim 9 or 10, characterized in that said diol comprises one or more of neopentyl glycol, 1, 4-butanediol, 1, 4-cyclohexanedimethanol, diethylene glycol, trimethylpentanediol, 2-methyl-1, 3-propanediol; the cross-linking agent comprises one or more than two of trimethylolpropane, trimethylolethane, tris (hydroxyethyl) isocyanurate and pentaerythritol; the catalyst is monobutyl tin oxide and/or dibutyl tin oxide; the antioxidant comprises one or more than two of antioxidant 1001, antioxidant 1010, antioxidant 1076, antioxidant 300 and antioxidant 168.
12. A method of preparing a matting heat transfer powder coating according to claim 8 characterised in that said curing agent is a β -hydroxyalkylamide; the leveling agent is selected from BLP503, the pigment filler comprises titanium dioxide, barium sulfate and/or barite, and the auxiliary agent is selected from benzoin.
13. The application of the extinction type thermal transfer powder coating of any one of claims 1 to 7 or the extinction type thermal transfer powder coating prepared by the preparation method of any one of claims 8 to 12 to the extinction type thermal transfer powder coating is characterized in that the extinction type thermal transfer powder coating is electrostatically sprayed on a metal plate which is degreased and descaled, and then the metal plate is placed into a 200 ℃ constant temperature oven to be cured for more than 10min to obtain the extinction type thermal transfer powder coating, and finally a transfer template is obtained through thermal transfer.
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