CN115124701B - Difunctional polyester resin, powder coating and application - Google Patents
Difunctional polyester resin, powder coating and application Download PDFInfo
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- CN115124701B CN115124701B CN202210956481.8A CN202210956481A CN115124701B CN 115124701 B CN115124701 B CN 115124701B CN 202210956481 A CN202210956481 A CN 202210956481A CN 115124701 B CN115124701 B CN 115124701B
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- 238000000576 coating method Methods 0.000 title claims abstract description 77
- 239000000843 powder Substances 0.000 title claims abstract description 77
- 239000011248 coating agent Substances 0.000 title claims abstract description 70
- 229920001225 polyester resin Polymers 0.000 title abstract description 38
- 239000004645 polyester resin Substances 0.000 title abstract description 38
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 67
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims abstract description 34
- 238000009835 boiling Methods 0.000 claims abstract description 14
- 239000000049 pigment Substances 0.000 claims abstract description 13
- ISAOCJYIOMOJEB-UHFFFAOYSA-N benzoin Chemical compound C=1C=CC=CC=1C(O)C(=O)C1=CC=CC=C1 ISAOCJYIOMOJEB-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 10
- 244000028419 Styrax benzoin Species 0.000 claims abstract description 6
- 235000000126 Styrax benzoin Nutrition 0.000 claims abstract description 6
- 235000008411 Sumatra benzointree Nutrition 0.000 claims abstract description 6
- 229960002130 benzoin Drugs 0.000 claims abstract description 6
- 235000019382 gum benzoic Nutrition 0.000 claims abstract description 6
- 238000005282 brightening Methods 0.000 claims abstract description 5
- 239000000126 substance Substances 0.000 claims abstract description 5
- 239000000463 material Substances 0.000 claims description 52
- 239000002253 acid Substances 0.000 claims description 36
- 238000010438 heat treatment Methods 0.000 claims description 27
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 24
- 229920005989 resin Polymers 0.000 claims description 21
- 239000011347 resin Substances 0.000 claims description 21
- OUPZKGBUJRBPGC-UHFFFAOYSA-N 1,3,5-tris(oxiran-2-ylmethyl)-1,3,5-triazinane-2,4,6-trione Chemical group O=C1N(CC2OC2)C(=O)N(CC2OC2)C(=O)N1CC1CO1 OUPZKGBUJRBPGC-UHFFFAOYSA-N 0.000 claims description 20
- 238000005886 esterification reaction Methods 0.000 claims description 20
- 238000000034 method Methods 0.000 claims description 19
- 238000001816 cooling Methods 0.000 claims description 15
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 14
- 239000000203 mixture Substances 0.000 claims description 14
- 239000012948 isocyanate Substances 0.000 claims description 13
- 150000002513 isocyanates Chemical class 0.000 claims description 13
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 claims description 12
- 239000011521 glass Substances 0.000 claims description 12
- QQVIHTHCMHWDBS-UHFFFAOYSA-N isophthalic acid Chemical compound OC(=O)C1=CC=CC(C(O)=O)=C1 QQVIHTHCMHWDBS-UHFFFAOYSA-N 0.000 claims description 12
- 239000000155 melt Substances 0.000 claims description 12
- 239000010445 mica Substances 0.000 claims description 12
- 229910052618 mica group Inorganic materials 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 229910052751 metal Inorganic materials 0.000 claims description 9
- 239000002184 metal Substances 0.000 claims description 9
- BVFSYZFXJYAPQJ-UHFFFAOYSA-N butyl(oxo)tin Chemical compound CCCC[Sn]=O BVFSYZFXJYAPQJ-UHFFFAOYSA-N 0.000 claims description 8
- SLCVBVWXLSEKPL-UHFFFAOYSA-N neopentyl glycol Chemical compound OCC(C)(C)CO SLCVBVWXLSEKPL-UHFFFAOYSA-N 0.000 claims description 8
- 235000006408 oxalic acid Nutrition 0.000 claims description 8
- QXJQHYBHAIHNGG-UHFFFAOYSA-N trimethylolethane Chemical compound OCC(C)(CO)CO QXJQHYBHAIHNGG-UHFFFAOYSA-N 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 7
- 229910052757 nitrogen Inorganic materials 0.000 claims description 7
- 238000007873 sieving Methods 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- 238000006068 polycondensation reaction Methods 0.000 claims description 6
- 239000004576 sand Substances 0.000 claims description 6
- 150000002148 esters Chemical class 0.000 claims description 5
- 238000001125 extrusion Methods 0.000 claims description 4
- 229910000861 Mg alloy Inorganic materials 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims 1
- 239000000945 filler Substances 0.000 abstract description 14
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 abstract description 6
- 239000001257 hydrogen Substances 0.000 abstract description 4
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 4
- 229920002521 macromolecule Polymers 0.000 abstract description 4
- 238000005507 spraying Methods 0.000 abstract description 2
- 238000002360 preparation method Methods 0.000 description 15
- 230000032050 esterification Effects 0.000 description 14
- 239000002245 particle Substances 0.000 description 10
- 239000006085 branching agent Substances 0.000 description 8
- 239000003054 catalyst Substances 0.000 description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 6
- 239000002994 raw material Substances 0.000 description 6
- 239000000853 adhesive Substances 0.000 description 5
- 230000001070 adhesive effect Effects 0.000 description 5
- 239000002671 adjuvant Substances 0.000 description 5
- 239000003963 antioxidant agent Substances 0.000 description 5
- 230000003078 antioxidant effect Effects 0.000 description 5
- 229920000728 polyester Polymers 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- 239000006097 ultraviolet radiation absorber Substances 0.000 description 5
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 4
- 230000008033 biological extinction Effects 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 4
- 239000006229 carbon black Substances 0.000 description 4
- 230000003068 static effect Effects 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 229910052788 barium Inorganic materials 0.000 description 3
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000003973 paint Substances 0.000 description 3
- 150000003384 small molecules Chemical class 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000004132 cross linking Methods 0.000 description 2
- 239000006224 matting agent Substances 0.000 description 2
- 239000004408 titanium dioxide Substances 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- YIMQCDZDWXUDCA-UHFFFAOYSA-N [4-(hydroxymethyl)cyclohexyl]methanol Chemical compound OCC1CCC(CO)CC1 YIMQCDZDWXUDCA-UHFFFAOYSA-N 0.000 description 1
- 239000006096 absorbing agent Substances 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000003242 anti bacterial agent Substances 0.000 description 1
- QRUDEWIWKLJBPS-UHFFFAOYSA-N benzotriazole Chemical compound C1=CC=C2N[N][N]C2=C1 QRUDEWIWKLJBPS-UHFFFAOYSA-N 0.000 description 1
- 239000012964 benzotriazole Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- XCJYREBRNVKWGJ-UHFFFAOYSA-N copper(II) phthalocyanine Chemical compound [Cu+2].C12=CC=CC=C2C(N=C2[N-]C(C3=CC=CC=C32)=N2)=NC1=NC([C]1C=CC=CC1=1)=NC=1N=C1[C]3C=CC=CC3=C2[N-]1 XCJYREBRNVKWGJ-UHFFFAOYSA-N 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 150000002009 diols Chemical class 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000005187 foaming Methods 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 238000002329 infrared spectrum Methods 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 230000020477 pH reduction Effects 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 230000003678 scratch resistant effect Effects 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 238000001196 time-of-flight mass spectrum Methods 0.000 description 1
- 239000005028 tinplate Substances 0.000 description 1
- 239000001038 titanium pigment Substances 0.000 description 1
- 239000010455 vermiculite Substances 0.000 description 1
- 229910052902 vermiculite Inorganic materials 0.000 description 1
- 235000019354 vermiculite Nutrition 0.000 description 1
- 239000002918 waste heat Substances 0.000 description 1
Classifications
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D1/00—Processes for applying liquids or other fluent materials
- B05D1/02—Processes for applying liquids or other fluent materials performed by spraying
- B05D1/04—Processes for applying liquids or other fluent materials performed by spraying involving the use of an electrostatic field
- B05D1/06—Applying particulate materials
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
- B05D7/14—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials to metal, e.g. car bodies
-
- 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
-
- 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
- C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
- C09D175/04—Polyurethanes
- C09D175/06—Polyurethanes from polyesters
-
- 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
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G2150/00—Compositions for coatings
- C08G2150/20—Compositions for powder coatings
Abstract
The invention discloses a difunctional polyester resin, a powder coating and application thereof, wherein the difunctional polyester resin with hydroxyl and carboxyl is matched with a first curing agent, a second curing agent, a first filler, a second filler, benzoin, a leveling agent, a brightening agent, a pigment, a boiling resistant agent and an auxiliary agent; compared with the common carboxyl-terminated polyester resin, the difunctional polyester resin in the obtained powder coating spray coating has better chemical resistance because more urethane bonds are introduced into molecules after curing, and has outstanding mechanical properties and higher hardness because hydrogen bonds are formed between macromolecules due to the existence of the urethane bonds.
Description
Technical Field
The invention relates to the technical field of powder coatings, in particular to a difunctional polyester resin, a powder coating and application.
Background
The coating is damaged in the outdoor extreme use process, and the conditions of foaming, falling off and the like appear. Therefore, the method has very important significance for improving the hardness, adhesive force, boiling resistance and the like of the powder coating, saving energy, reducing emission and prolonging the service life of the material. Polyester resins are key to optimizing outdoor system powder coatings as an important component of powder coatings.
The invention discloses a high-hardness polyester resin powder coating, which comprises, by weight, 50-60 parts of saturated carboxyl-terminated polyester resin, 6-10 parts of triglycidyl isocyanurate, 1-2 parts of beta-hydroxyalkylamide, 1-2 parts of iron oxide red, 0.1-1 part of titanium dioxide, 1-2 parts of benzotriazole, 5-10 parts of vermiculite powder, 1-2 parts of sodium fluosilicate, 1, 4-cyclohexanedimethanol and 7-10 parts of composite filler.
The structure and curing reaction principle of the difunctional polyester resin are analyzed in the paint industry 2019 49 (03), and the influence of the acid value and the hydroxyl value of the difunctional polyester resin, the matting agent and the type and the content of the filler on the matting performance of the powder coating in the powder paint formula is studied. The results show that the extinction gloss of the coating is increased along with the increase of the acid value of the difunctional polyester resin, the change of the hydroxyl value of the difunctional polyester resin has less influence on the extinction gloss of the coating, and when the extinction curing agent is used, the extinction effect of the filler adopting high-gloss barium and precipitated barium is more excellent.
Coating industry 2021 51 (09): 15-19 article analysis to investigate the effect of curing agent types and combinations thereof on the anti-bloom properties of a coating, powder coatings were prepared using the same difunctional resin (containing 2 functional groups of carboxyl and hydroxyl groups) in combination with triglycidyl isocyanurate (TGIC), beta-Hydroxyalkylamide (HAA), epoxy resin (E12) and isocyanate (B1530). And (3) placing the coating in an oven to perform baking experiments at different temperatures and times, and analyzing white frost by using infrared spectrum and time-of-flight mass spectrum with the light retention as a basis for judging the frosting degree of the coating. The result shows that when the coating is cured, the lower curing speed and the lower crosslinking density of the coating are beneficial to timely discharging small molecules in the coating, the residual quantity of the small molecules in the coating is reduced, the crosslinking density of the coating is increased, the residual small molecules in the coating are coated, the frosting phenomenon under the action of waste heat is improved, and the initial experimental result shows that the migration degree of white frost from the coating to the surface of the coating is obviously increased when the temperature is more than 120 ℃, and the white frost is easy to desorb from the surface of the coating after the temperature is more than 160 ℃.
Aiming at the defects and the shortcomings of the existing powder coating, it is necessary to find an outdoor powder coating product with excellent comprehensive performance and proper cost.
Disclosure of Invention
The invention provides a preparation method of a difunctional polyester resin, and the difunctional polyester resin prepared by the invention can enhance the adhesive force and hardness of a coating of a paint and improve the performance of the coating.
In order to solve the technical problem, the technical scheme of the invention is as follows: a method for preparing a difunctional polyester resin, comprising the following steps:
firstly, taking dihydric alcohol and a branching agent, and heating until materials are melted;
adding dibasic acid and esterification catalyst, introducing nitrogen, continuously heating to react until the esterification water is generated and distilled off at 170-180 ℃, gradually heating to 230-255 ℃ after 8-10 h, and preserving heat at the temperature for 2-4 h until the material system is clear and transparent;
step three, cooling to 200-210 ℃, and vacuumizing for 3-5 hours, wherein the acid value of the material is below 15mgKOH/g, and the hydroxyl value is 55-95 mgKOH/g;
continuously heating to 228-236 ℃, adding an acidolysis agent, and reacting for 3-5 hours until a material system is clear and transparent, wherein the acid value reaches 30-55 mgKOH/g, and the hydroxyl value is 40-55 mgKOH/g;
and fifthly, cooling to 220-226 ℃, vacuumizing, polycondensing for 1-1.5 h, wherein the acid value reaches 10-56 mgKOH/g, and the hydroxyl value reaches 33-53 mgKOH/g, thus obtaining the difunctional polyester resin.
The preferred preparation raw materials comprise the following components in parts by mass:
45 to 55 parts of dihydric alcohol; 0.1 to 0.5 parts of branching agent;
40-50 parts of dibasic acid; 0.05 to 1.0 part of an esterification catalyst;
5 to 10 parts of acidolysis agent.
Preferably the diol is neopentyl glycol; the branching agent is trimethylolethane; the dibasic acid is oxalic acid; the esterification catalyst is monobutyl tin oxide; the acidolysis agent is isophthalic acid and/or terephthalic acid.
The second purpose of the invention is to provide a powder coating, which can effectively improve the hardness, adhesive force and boiling resistance of the obtained coating.
In order to solve the technical problem, the technical scheme of the invention is as follows: the powder coating comprises the following substances in percentage by mass:
45 to 80 percent of the difunctional agglomerated ester resin prepared by the invention;
2.4% to 6.0% of a first curing agent;
3.4% to 15% of a second curing agent;
5% to 40% of a first filler;
5% to 40% of a second filler;
benzoin 0.1% to 0.5%;
0.1 to 1.5 percent of leveling agent;
0.1 to 1.5% of brightening agent;
pigment 0.8% to 25%;
0.5 to 1.5 percent of boiling resistant agent
0.8 to 1.2 percent of auxiliary agent.
Preferably also comprises according to mass fraction
Sand grain agent 0.05-1.0%;
0.1 to 2.0 percent of wax powder.
The sand grain agent is an auxiliary agent for producing sand grain powder coating, and the wax powder has the functions of defoaming, scratch resistance and the like.
Preferably, the first curing agent is triglycidyl isocyanurate and the second curing agent is a blocked isocyanate.
The curing process comprises the following steps:
step one, deblocking blocked isocyanate;
step two, reacting the deblocked isocyanate with the hydroxyl of the difunctional coacervate resin;
triglycidyl isocyanurate (TGIC) is reacted with carboxyl groups of the difunctional coacervate resin;
finally, the target product is crosslinked, and the specific reaction route is shown in figure 1.
Compared with the common carboxyl-terminated polyester resin, the difunctional polyester resin has good chemical resistance because more urethane bonds are introduced into molecules after curing, and has outstanding mechanical properties and higher hardness because hydrogen bonds are formed between macromolecules due to the existence of the urethane bonds.
Preferably, the first filler is a glass frit; the second filler is mica powder. The invention adopts double fillers to improve the curing effect of the coating.
The third object of the invention is to provide a preparation method of the powder coating, which has simple preparation process, and the obtained powder coating is suitable for being coated on the metal surface.
In order to solve the technical problem, the technical scheme of the invention is as follows: a method for preparing a powder coating, comprising the steps of:
step one, placing the components in a mixing cylinder according to the mass fraction, and stirring for 3-6min to obtain a mixture;
step two, placing the mixture obtained in the step one in a melt extruder to extrude at the temperature of 80-120 ℃ to obtain an extrusion material;
and thirdly, crushing the extrusion material in the second step, and sieving to obtain a powder finished product with the D50 of 32-38 microns.
The fourth object of the invention is to provide an application of the powder coating, which is suitable for spraying on the metal surface, and can effectively improve the hardness, the adhesive force and the boiling resistance of the obtained coating.
In order to solve the technical problem, the technical scheme of the invention is as follows: a film forming method for metal surface is to coat the powder coating on the surface of metal product by high-voltage electrostatic method.
Preferably, the metal product is a magnesium alloy product. The magnesium alloy product is used as a light structural material and has the characteristics of small density, high strength, good toughness and the like.
The preferred coating process parameters are as follows:
the high-voltage static electricity is 60-90KV;
the thickness of the coating film is 50-120 micrometers;
the curing temperature is 180-200 ℃;
the curing time is 10-20 minutes.
The preferred coating process parameters are as follows:
the thickness of the coating film is 60-90 micrometers;
the curing temperature is 190-200 ℃;
the curing time is 10-15 minutes.
The film forming process ensures complete solidification of the outdoor difunctional agglomerated ester powder coating, and has proper coating thickness and optimal performance.
By adopting the technical scheme, the invention has the beneficial effects that:
based on difunctional agglomerate resin, a first curing agent, a second curing agent, glass powder, mica powder double-filler, a brightening agent, a delustering agent, an antioxidant, an antibacterial agent, an ultraviolet absorber, a deaerating agent, a scratch resistant agent and other auxiliary agents are matched to form a basic formula;
the hydroxyl and carboxyl of the difunctional polyester resin react with the first curing agent and the second curing agent respectively for curing, so that more urethane bonds are introduced in the presence of the first curing agent, hydrogen bonds are formed among macromolecules due to the presence of the urethane bonds, and the difunctional polyester resin can enhance the adhesive force and hardness of the coating.
Drawings
FIG. 1 is a schematic illustration of the curing process of the difunctional coacervate ester resin proposed in the present invention;
FIG. 2 is a schematic illustration of the powder coating of the present invention formed into a film without bubbles;
FIG. 3 is a graph showing the formation of slight bubbles after film formation of the powder coating material of the present invention;
FIG. 4 shows the formation of severe bubbles after film formation of the powder coating material according to the invention.
Detailed Description
In order to further explain the technical scheme of the invention, the invention is explained in detail by specific examples.
Example 1
The embodiment discloses a difunctional polyester powder coating which comprises the following components in percentage by mass: 60% of a difunctional coacervate resin; 4.6% of a curing agent TGIC (triglycidyl isocyanurate); 11% of curing agent NW-5 (blocked isocyanate), 9% of glass powder and 7.5% of mica powder; 1% of a boiling resistant agent W-5322 and 1.0% of a leveling agent GLP588;0.6% brightener 701B; benzoin 0.3%;4.2% pigment; 0.8% of an auxiliary agent;
the difunctional coacervate resin in this example was an acid value of 25mgKOH/g and a hydroxyl value of 35mgKOH/g. The preparation method of the difunctional polyester resin specifically comprises the following steps:
step one, taking 45 parts by mass of dihydric alcohol (neopentyl glycol) and 0.2 part by mass of branching agent (trimethylolethane), and heating until materials are melted;
adding 40 parts by mass of dibasic acid (oxalic acid) and 0.06 part by mass of esterification catalyst (monobutyl tin oxide), introducing nitrogen, continuously heating to react (esterification reaction), starting to generate and distillate esterification water at 180 ℃, gradually heating to 230 ℃ after 10 hours, and preserving heat at the temperature for 3 hours until a material system is clear and transparent;
step three, cooling to 210 ℃, and vacuumizing for 5 hours, wherein the acid value of the material is lower than 15mgKOH/g, and the hydroxyl value is 55mgKOH/g;
continuously heating to 230 ℃, adding 5 parts by mass of acidolysis agent, which is isophthalic acid in the embodiment, and performing polycondensation reaction for 5 hours until a material system is clear and transparent, wherein the acid value reaches 30KOH/g and the hydroxyl value is 40mgKOH/g;
and fifthly, cooling to 220 ℃, vacuumizing, polycondensing for 1.5 hours, wherein the acid value reaches 25mgKOH/g, and the hydroxyl value reaches 35mgKOH/g, thus obtaining the difunctional polyester resin.
The pigment in this example comprises 3.0% titanium dioxide; 0.5% phthalocyanine blue; 0.7% iron oxide yellow;
the adjuvants in this example include 0.5% antioxidant 626;0.3% of ultraviolet absorber.
The specific preparation method of the powder coating in the embodiment is as follows:
(1) Placing the raw materials with the dosage of the formula above a mixing cylinder and stirring for 6min to obtain a mixture;
(2) Extruding the mixture obtained in the step (1) in a melt extruder at 120 ℃ to obtain an extruded material; the melt extruder is a double-screw or single-screw extruder;
(3) And (3) putting the extruded material obtained in the step (2) into a vertical mill for crushing, and then sieving the crushed material with a 180-mesh sieve to prepare a powder finished product with the particle size (equivalent particle size D50) of 32-38 microns for later use.
The powder coating prepared by the preparation method is coated on the surface of a tin product by a high-voltage static method, wherein the high-voltage static is 60-90KV high-voltage static, the average coating thickness is 50-120 micrometers, the curing temperature is 180-200 ℃, the curing time is 10-20 minutes, and the powder coating can be cured by an oven or infrared rays. Preferably, the average coating film thickness is 60-90 micrometers, the curing temperature is 190-200 ℃, and the curing time is 10-15 minutes.
Example 2
The embodiment discloses a difunctional polyester powder coating which comprises the following components in percentage by mass: 65% of a difunctional coacervate resin; 5% of a curing agent TGIC (triglycidyl isocyanurate); 8% of curing agent NW-5 (blocked isocyanate), 9.5% of glass powder and 7.5% of mica powder; 1% of a boiling resistant agent W-5322 and 1.0% of a leveling agent GLP588;0.6% brightener 701B; benzoin 0.4%;1.0% pigment; 1.0% of an auxiliary agent;
the difunctional coacervate resin in this example was an acid value of 20mgKOH/g and a hydroxyl value of 35mgKOH/g. The preparation method of the difunctional polyester resin specifically comprises the following steps:
step one, taking 45 parts by mass of dihydric alcohol (neopentyl glycol) and 0.1 part by mass of branching agent (trimethylolethane), and heating until materials are melted;
adding 35 parts by mass of dibasic acid (oxalic acid) and 0.06 part by mass of esterification catalyst (monobutyl tin oxide), introducing nitrogen, continuously heating to react (esterification reaction), starting to generate and distillate esterification water at 180 ℃, gradually heating to 230 ℃ after 10 hours, and preserving heat at the temperature for 3 hours until a material system is clear and transparent;
step three, cooling to 210 ℃, and vacuumizing for 5 hours, wherein the acid value of the material is lower than 10mgKOH/g, and the hydroxyl value is 55mgKOH/g;
continuously heating to 230 ℃, adding 5 parts by mass of acidolysis agent, namely terephthalic acid in the embodiment, and performing polycondensation reaction for 5 hours until a material system is clear and transparent, wherein the acid value reaches 25mgKOH/g and the hydroxyl value reaches 40mgKOH/g;
and fifthly, cooling to 220 ℃, vacuumizing, polycondensing for 1.5 hours, wherein the acid value reaches 20mgKOH/g, and the hydroxyl value reaches 35mgKOH/g, thus obtaining the difunctional polyester resin.
The pigment in this example is carbon black;
the adjuvants in this example included 0.5% uv absorber, 0.5% wax powder.
The specific preparation method of the powder coating in the embodiment is as follows:
(1) Placing the raw materials with the dosage of the formula above a mixing cylinder and stirring for 6min to obtain a mixture;
(2) Extruding the mixture obtained in the step (1) in a melt extruder at 120 ℃ to obtain an extruded material; the melt extruder is a double-screw or single-screw extruder;
(3) And (3) putting the extruded material obtained in the step (2) into a vertical mill for crushing, and then sieving the crushed material with a 180-mesh sieve to prepare a powder finished product with the particle size (equivalent particle size D50) of 32-38 microns for later use.
The procedure is as in example 1.
Example 3
The embodiment discloses a difunctional polyester powder coating which comprises the following components in percentage by mass: 65% of a difunctional coacervate resin; 5% of a curing agent TGIC (triglycidyl isocyanurate); 5% of curing agent NW-5 (blocked isocyanate), 1% of boiling resistant agent W-5322, 10% of glass powder and 9% of mica powder; 1% of boiling resistant agent W-5322 and 0.4% of sand grain agent; 2.4% pigment; 1.2% of an auxiliary agent;
the difunctional coacervate resin in this example was of acid value 25mgKOH/g and hydroxyl value 45mgKOH/g. The preparation method of the difunctional polyester resin specifically comprises the following steps:
step one, taking 48 parts by mass of dihydric alcohol (neopentyl glycol) and 0.1 part by mass of branching agent (trimethylolethane), and heating until materials are melted;
adding 40 parts by mass of dibasic acid (oxalic acid) and 0.06 part by mass of esterification catalyst (monobutyl tin oxide), introducing nitrogen, continuously heating to react (esterification reaction), starting to generate and distillate esterification water at 180 ℃, gradually heating to 230 ℃ after 10 hours, and preserving heat at the temperature for 3 hours until a material system is clear and transparent;
step three, cooling to 210 ℃, and vacuumizing for 5 hours, wherein the acid value of the material is lower than 10mgKOH/g, and the hydroxyl value is 55mgKOH/g;
continuously heating to 230 ℃, adding 6 parts by mass of acidolysis agent, wherein the acidolysis agent is mixed with isophthalic acid and terephthalic acid with equal mass in the embodiment, and carrying out polycondensation reaction for 5 hours until a material system is clear and transparent, wherein the acid value reaches 30mgKOH/g, and the hydroxyl value is 50mgKOH/g;
and fifthly, cooling to 220 ℃, vacuumizing, polycondensing for 1.5 hours, wherein the acid value reaches 25mgKOH/g, and the hydroxyl value reaches 45mgKOH/g, thus obtaining the difunctional polyester resin.
The pigment in this example is carbon black;
the adjuvants in this example included 0.5% antioxidant, 0.3% ultraviolet absorber and 0.4% wax powder.
The specific preparation method of the powder coating in the embodiment is as follows:
(1) Placing the raw materials with the dosage of the formula above a mixing cylinder and stirring for 6min to obtain a mixture;
(2) Extruding the mixture obtained in the step (1) in a melt extruder at 120 ℃ to obtain an extruded material; the melt extruder is a double-screw or single-screw extruder;
(3) And (3) putting the extruded material obtained in the step (2) into a vertical mill for crushing, and then sieving the crushed material with a 180-mesh sieve to prepare a powder finished product with the particle size (equivalent particle size D50) of 32-38 microns for later use.
The procedure is as in example 1.
Example 4
The difunctional polyester powder coating comprises the following components in percentage by mass: 70% of a difunctional coacervate resin; 5.5% curative TGIC;8.5% of curing agent NW-5 (blocked isocyanate), 4% of glass powder and 3.7% of mica powder; 1% of a boiling resistant agent W-5322 and 1.0% of a leveling agent GLP588;3% matting agent; 0.8 brightening agent, 0.5 benzoin; 0.8% pigment; 1.2% of an auxiliary agent;
the difunctional coacervate resin in this example was 45mgKOH/g acid value and 40mgKOH/g hydroxyl value. The preparation method of the difunctional polyester resin specifically comprises the following steps:
step one, taking 40 parts by mass of dihydric alcohol (neopentyl glycol) and 0.2 part by mass of branching agent (trimethylolethane), heating and raising the temperature until materials are melted;
adding 45 parts by mass of dibasic acid (oxalic acid) and 0.7 part by mass of esterification catalyst (monobutyl tin oxide), introducing nitrogen, continuously heating to react (esterification reaction), starting to generate and distillate esterification water at 180 ℃, gradually heating to 230 ℃ after 10 hours, and preserving heat at the temperature for 3 hours until a material system is clear and transparent;
step three, cooling to 210 ℃, and vacuumizing for 5 hours, wherein the acid value of the material is lower than 20mgKOH/g, and the hydroxyl value is 55mgKOH/g;
continuously heating to 230 ℃, adding 8 parts by mass of acidolysis agent, namely isophthalic acid, carrying out polycondensation reaction for 5 hours until a material system is clear and transparent, wherein the acid value reaches 50mgKOH/g, and the hydroxyl value is 45mgKOH/g;
and fifthly, cooling to 220 ℃, vacuumizing, polycondensing for 1.5 hours, wherein the acid value reaches 45mgKOH/g, and the hydroxyl value reaches 40mgKOH/g, thus obtaining the difunctional polyester resin.
The pigment in this example is carbon black;
the adjuvants in this example included 0.5% antioxidant, 0.3% ultraviolet absorber and 0.4% wax powder.
The specific preparation method of the powder coating in the embodiment is as follows:
(1) Placing the raw materials with the dosage of the formula above a mixing cylinder and stirring for 6min to obtain a mixture;
(2) Extruding the mixture obtained in the step (1) in a melt extruder at 120 ℃ to obtain an extruded material; the melt extruder is a double-screw or single-screw extruder;
(3) And (3) putting the extruded material obtained in the step (2) into a vertical mill for crushing, and then sieving the crushed material with a 180-mesh sieve to prepare a powder finished product with the particle size (equivalent particle size D50) of 32-38 microns for later use.
The procedure is as in example 1.
Example 5
The embodiment discloses a difunctional polyester powder coating which comprises the following components in percentage by mass: 65% of a difunctional coacervate resin; 5% of a curing agent TGIC (triglycidyl isocyanurate); 8% of a curing agent NW-5 (blocked isocyanate); 1% of boiling resistant agent W-5322 and 0.4% of sand grain agent; 6% of glass powder and 5% of mica powder; 8.4% pigment; 1.2% of an auxiliary agent;
the difunctional coacervate resin in this example was an acid value of 20mgKOH/g and a hydroxyl value of 45mgKOH/g. The preparation method of the difunctional polyester resin specifically comprises the following steps:
step one, taking 45 parts by mass of dihydric alcohol (neopentyl glycol) and 0.1 part by mass of branching agent (trimethylolethane), and heating until materials are melted;
adding 35 parts by mass of dibasic acid (oxalic acid) and 0.06 part by mass of esterification catalyst (monobutyl tin oxide), introducing nitrogen, continuously heating to react (esterification reaction), starting to generate and distillate esterification water at 180 ℃, gradually heating to 230 ℃ after 10 hours, and preserving heat at the temperature for 3 hours until a material system is clear and transparent;
step three, cooling to 210 ℃, and vacuumizing for 5 hours, wherein the acid value of the material is lower than 15mgKOH/g, and the hydroxyl value is 55mgKOH/g;
continuously heating to 230 ℃, adding 6 parts by mass of acidolysis agent, namely terephthalic acid, and performing polycondensation reaction for 5 hours until a material system is clear and transparent, wherein the acid value reaches 25mgKOH/g and the hydroxyl value is 50mgKOH/g;
and fifthly, cooling to 220 ℃, vacuumizing, polycondensing for 1.5 hours, wherein the acid value reaches 20mgKOH/g, and the hydroxyl value reaches 45mgKOH/g, thus obtaining the difunctional polyester resin.
The pigments in this embodiment are carbon black and titanium pigment;
the adjuvants in this example included 0.5% antioxidant, 0.3% ultraviolet absorber and 0.4% wax powder.
The specific preparation method of the powder coating in the embodiment is as follows:
(1) Placing the raw materials with the dosage of the formula above a mixing cylinder and stirring for 6min to obtain a mixture;
(2) Extruding the mixture obtained in the step (1) in a melt extruder at 120 ℃ to obtain an extruded material; the melt extruder is a double-screw or single-screw extruder;
(3) And (3) putting the extruded material obtained in the step (2) into a vertical mill for crushing, and then sieving the crushed material with a 180-mesh sieve to prepare a powder finished product with the particle size (equivalent particle size D50) of 32-38 microns for later use.
The procedure is as in example 1.
Comparative example 1
The only difference from example 1 is that the difunctional polyester resin is replaced by an equivalent amount of carboxyl terminated polyester resin and the curing agent TGIC is used for curing.
Comparative example 2
The only difference from example 1 is that the difunctional polyester resin is replaced with an equivalent amount of hydroxyl terminated polyester resin and the curing agent NW-5 is used for curing.
Comparative example 3
The only difference from example 4 is that the double filler glass frit and mica powder are replaced with equal amounts of glass frit.
Comparative example 4
The only difference from example 5 is that the double filler glass frit and mica powder are replaced with equal amounts of mica powder.
Comparative example 5
The only difference from example 2 is that the double filler glass frit and mica powder are replaced with an equal amount of precipitated barium.
Performance test: the coatings of each example were subjected to performance testing, and specific test data are shown in Table 1. The water boiling test comprises the steps of completely putting a sample into hot water, boiling the sample in the hot water for 30min, taking out the sample, and cooling the sample to the normal temperature. Specifically, each coating was sprayed onto a flat tinplate so that the thickness of the dried coating film was 0.1mm, and then the coating film was placed in each of the rolls for 30 minutes, and after completion, the surface condition of the coating film was observed and an adhesion test was performed.
Table 1 properties of the film layers obtained in examples 1 to 5 and comparative examples 1 to 5
As can be seen from the comparison of the performance indexes in table 1, the first curing agent is triglycidyl isocyanurate, the second curing agent is blocked isocyanate, and the following steps are included in the curing process:
step one, deblocking blocked isocyanate;
step two, reacting the deblocked isocyanate with the hydroxyl of the difunctional coacervate resin;
triglycidyl isocyanurate (TGIC) is reacted with carboxyl groups of the difunctional coacervate resin;
finally, the target product is crosslinked, and the specific reaction route is shown in figure 1.
Compared with the common carboxyl-terminated polyester resin, the difunctional polyester resin has good chemical resistance because more urethane bonds are introduced into molecules after curing, and has outstanding mechanical properties and higher hardness because hydrogen bonds are formed between macromolecules due to the existence of the urethane bonds.
Claims (6)
1. A powder coating, characterized by: the material comprises the following substances in percentage by mass:
45% to 80% of a difunctional coacervate resin;
2.4% to 6.0% of a first curing agent;
3.4% to 15% of a second curing agent;
5% to 40% of glass frit;
5% to 40% of mica powder;
benzoin 0.1% to 0.5%;
0.1 to 1.5 percent of leveling agent;
0.1 to 1.5% of brightening agent;
pigment 0.8% to 25%;
0.5 to 1.5 percent of boiling resistant agent
0.8 to 1.2 percent of auxiliary agent;
the difunctional coacervate ester resin is prepared by the following steps:
step one, neopentyl glycol and trimethylolethane are taken, heated and warmed until materials are melted;
adding oxalic acid and monobutyl tin oxide, introducing nitrogen, continuously heating to perform esterification reaction, starting to generate and distillate esterified water at 170-180 ℃, gradually heating to 230-255 ℃ after 8-10 h, and preserving heat at the temperature for 2-4 h until a material system is clear and transparent;
step three, cooling to 200-210 ℃, and vacuumizing for 3-5 hours, wherein the acid value of the material is below 15mgKOH/g, and the hydroxyl value is 55-95 mgKOH/g;
continuously heating to 228-236 ℃, adding 5-10% of isophthalic acid and/or terephthalic acid, and performing polycondensation reaction for 3-5 hours until a material system is clear and transparent, wherein the acid value reaches 30-55 mgKOH/g and the hydroxyl value is 40-55 mgKOH/g;
fifthly, cooling to 220-226 ℃, vacuumizing and polycondensing for 1-1.5 h, wherein the acid value reaches 10-56 mgKOH/g, and the hydroxyl value reaches 33-53 mgKOH/g, thus obtaining the difunctional coacervate ester resin;
45 parts to 55 parts of neopentyl glycol; 0.1 to 0.5 part of trimethylolethane;
40 to 50 parts of oxalic acid; 0.05 to 1.0 part of monobutyl tin oxide;
5 to 10 parts of isophthalic acid and/or terephthalic acid.
2. A powder coating as recited in claim 1, wherein:
also comprises according to mass fraction
Sand grain agent 0.05-1.0%;
0.1 to 2.0 percent of wax powder.
3. A powder coating as recited in claim 1, wherein: the first curing agent is triglycidyl isocyanurate and the second curing agent is blocked isocyanate.
4. A process for preparing a powder coating as claimed in any one of claims 1 to 3, wherein: the method comprises the following steps:
step one, placing the components in a mixing cylinder according to the mass fraction, and stirring for 3-6min to obtain a mixture;
step two, placing the mixture obtained in the step one in a melt extruder to extrude at the temperature of 80-120 ℃ to obtain an extrusion material;
and thirdly, crushing the extrusion material in the second step, and sieving to obtain a powder finished product with the D50 of 32-38 microns.
5. A film forming method for a metal surface is characterized in that: a powder coating according to any one of claims 1 to 3 applied to the surface of a metal product by a high-voltage electrostatic method.
6. The method for forming a film on a metal surface according to claim 5, wherein: the metal product is a magnesium alloy product.
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