CN115926603A - Anti-bending transparent matte high-hardness powder coating and preparation method thereof - Google Patents
Anti-bending transparent matte high-hardness powder coating and preparation method thereof Download PDFInfo
- Publication number
- CN115926603A CN115926603A CN202211441179.5A CN202211441179A CN115926603A CN 115926603 A CN115926603 A CN 115926603A CN 202211441179 A CN202211441179 A CN 202211441179A CN 115926603 A CN115926603 A CN 115926603A
- Authority
- CN
- China
- Prior art keywords
- parts
- powder coating
- reaction kettle
- weight
- polyester resin
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000000843 powder Substances 0.000 title claims abstract description 135
- 238000000576 coating method Methods 0.000 title claims abstract description 126
- 239000011248 coating agent Substances 0.000 title claims abstract description 120
- 238000005452 bending Methods 0.000 title claims abstract description 53
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 229920001225 polyester resin Polymers 0.000 claims abstract description 75
- 239000004645 polyester resin Substances 0.000 claims abstract description 75
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 52
- 239000012948 isocyanate Substances 0.000 claims abstract description 22
- 150000002513 isocyanates Chemical class 0.000 claims abstract description 22
- 239000004593 Epoxy Substances 0.000 claims abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 19
- 239000011521 glass Substances 0.000 claims abstract description 18
- 238000007872 degassing Methods 0.000 claims abstract description 16
- 239000000463 material Substances 0.000 claims description 60
- 238000003756 stirring Methods 0.000 claims description 20
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 16
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 claims description 16
- 238000010438 heat treatment Methods 0.000 claims description 16
- QQVIHTHCMHWDBS-UHFFFAOYSA-N isophthalic acid Chemical compound OC(=O)C1=CC=CC(C(O)=O)=C1 QQVIHTHCMHWDBS-UHFFFAOYSA-N 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 12
- 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 11
- 238000002844 melting Methods 0.000 claims description 9
- 230000008018 melting Effects 0.000 claims description 9
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 claims description 8
- NPAIMXWXWPJRES-UHFFFAOYSA-N butyltin(3+) Chemical compound CCCC[Sn+3] NPAIMXWXWPJRES-UHFFFAOYSA-N 0.000 claims description 8
- 239000002245 particle Substances 0.000 claims description 5
- 229910000831 Steel Inorganic materials 0.000 claims description 4
- 235000011037 adipic acid Nutrition 0.000 claims description 4
- 239000001361 adipic acid Substances 0.000 claims description 4
- 239000003963 antioxidant agent Substances 0.000 claims description 4
- 230000003078 antioxidant effect Effects 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- SLCVBVWXLSEKPL-UHFFFAOYSA-N neopentyl glycol Chemical compound OCC(C)(C)CO SLCVBVWXLSEKPL-UHFFFAOYSA-N 0.000 claims description 4
- 238000007873 sieving Methods 0.000 claims description 4
- 239000010959 steel Substances 0.000 claims description 4
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 8
- 230000008569 process Effects 0.000 abstract description 8
- 238000012360 testing method Methods 0.000 description 8
- 239000011247 coating layer Substances 0.000 description 5
- 239000003973 paint Substances 0.000 description 5
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 4
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 4
- 229910052731 fluorine Inorganic materials 0.000 description 4
- 239000011737 fluorine Substances 0.000 description 4
- 239000011256 inorganic filler Substances 0.000 description 4
- 229910003475 inorganic filler Inorganic materials 0.000 description 4
- 238000004132 cross linking Methods 0.000 description 3
- 239000002966 varnish Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 230000006750 UV protection Effects 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000007590 electrostatic spraying Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 125000003700 epoxy group Chemical group 0.000 description 1
- 230000009477 glass transition Effects 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000004224 protection Effects 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
Landscapes
- Paints Or Removers (AREA)
Abstract
The invention discloses an anti-bending transparent matte high-hardness powder coating, which belongs to the technical field of powder coatings and comprises hydroxyl-terminated polyester resin, carboxyl-terminated polyester resin, blocked isocyanate, an epoxy curing agent, a flatting agent, a degassing agent and transparent glass micropowder. The invention also discloses a preparation method of the anti-bending transparent matte high-hardness powder coating, the prepared powder coating is sprayed on the surface of a workpiece, and the powder coating is cured to form a powder coating, and the obtained powder coating has the characteristics of high hardness and scratch resistance, proper flexibility and strong impact resistance, so that the product sprayed with the powder coating can be conveniently processed, and the appearance damage caused by collision in the using process of the product can be reduced. In addition, the powder coating is a matte transparent coating, can be used for a lighting layer, and not only does not influence the color effect of the primer, but also does not influence the aesthetic measure of the product due to scratches on the surface of the powder coating.
Description
Technical Field
The invention relates to the technical field of powder coatings, and particularly relates to an anti-bending transparent matte high-hardness powder coating and a preparation method thereof.
Background
The powder coating does not use a solvent, exists in a fine powder state, has the utilization rate of almost 100 percent in the using process, and has the advantages of harmlessness, high efficiency, resource saving, environmental protection and the like to replace the traditional solvent-based coating in a large area.
However, the conventional powder coating has the problems of low surface hardness and low scratch resistance when used, and has poor use effect in some occasions, such as public area tables and chairs, guardrails and the like. The hardness of the powder coating is usually below 1H, so that the fluorine-containing wax organic component and the hard inorganic filler are added into the powder coating to further improve the hardness of the powder coating, but the fluorine-containing wax organic component and the hard inorganic filler do not participate in reaction in the process of curing the powder coating, so that the powder coating is brittle and easy to crack when the hardness of the powder coating is above 3H, and has poor flexibility, and the requirements of workpiece bending and impact resistance in use cannot be met. In addition, when the gloss of the powder coating is high, scratches on the powder coating are significantly reflected, which may affect the aesthetic appearance of the product.
It is seen that improvements and enhancements in the prior art are needed.
Disclosure of Invention
In view of the defects of the prior art, the invention aims to provide an anti-bending transparent matte high-hardness powder coating and a preparation method thereof, and aims to solve the problem that the hardness and the flexibility of a powder coating cannot be simultaneously considered due to the addition of a fluorine-containing wax organic component and a hard inorganic filler in the powder coating and eliminate the influence of high glossiness of the powder coating on the attractiveness of a product.
In order to achieve the purpose, the invention adopts the following technical scheme:
an anti-bending transparent matte high-hardness powder coating comprises the following components in parts by weight; 130-200 parts of hydroxyl-terminated polyester resin, 130-210 parts of carboxyl-terminated polyester resin, 220-280 parts of blocked isocyanate, 10-25 parts of epoxy curing agent, 10 parts of flatting agent, 5 parts of degassing agent and 340 parts of transparent glass micro powder.
In the anti-bending transparent matte high-hardness powder coating, the ratio of the hydroxyl-terminated polyester resin to the carboxyl-terminated polyester resin is 1: 0.75-1.5 in parts by weight.
In the anti-bending transparent matte high-hardness powder coating, the ratio of the hydroxyl-terminated polyester resin to the blocked isocyanate in parts by weight is 1: 1.5.
In the anti-bending transparent matte high-hardness powder coating, the ratio of the carboxyl-terminated polyester resin to the epoxy curing agent is (8.5-9) to 1.5 in parts by weight.
In the anti-bending transparent matte high-hardness powder coating, the epoxy curing agent is triglycidyl isocyanurate.
The invention also provides a preparation method of the anti-bending transparent matte high-hardness powder coating, which comprises the following steps:
s001, adding hydroxyl-terminated polyester resin, carboxyl-terminated polyester resin, closed isocyanate, an epoxy curing agent, a flatting agent, a degassing agent and transparent glass micro powder into a mixer for premixing;
s002, melting and extruding the premixed material in the step S001 through an extruder;
s003, cooling and tabletting the melt-extruded material by using a water-cooled steel belt;
and S004, crushing the flaky material in the step S003 by a crusher, and sieving to obtain the anti-bending transparent matte high-hardness powder coating.
Further, in step S002, the temperature of the feed port of the extruder was 65 ℃ and the temperature of the melt zone was 105 ℃.
Further, in step S004, the particle size of the anti-bending transparent matte high-hardness powder coating is 30 to 50um.
Further, in step S001, the method for preparing the hydroxyl-terminated polyester resin comprises the steps of:
step A001, adding 2500 parts by weight of trihydroxypropane and 4 parts by weight of monobutyltin into a reaction kettle connected with a condensing tower, slowly heating the reaction kettle to 150 ℃, and stirring to dissolve the trihydroxypropane;
step A002, slowly adding 1000 parts by weight of terephthalic acid and 1600 parts by weight of isophthalic acid into a trihydroxypropane solution, and continuously stirring until the materials in the reaction kettle are uniformly dispersed;
step A003, after the materials in the reaction kettle are uniformly dispersed, slowly heating the reaction kettle to 240 ℃, and then keeping the temperature at the top end of a condensing tower below 101 ℃ to distill off water generated in the material reaction;
and step A004, after water generated in the material reaction is distilled off, continuously keeping the temperature of the reaction kettle at 240 ℃, reducing the temperature of the top end of the condensing tower to 50 ℃, starting a vacuum pump, and carrying out negative pressure reaction on the materials in the reaction kettle for 1 hour to obtain the hydroxyl-terminated polyester resin.
Further, in step S001, the method for preparing the carboxyl group terminated polyester resin comprises the steps of:
b001, adding 1260 parts by weight of neopentyl glycol, 300 parts by weight of ethylene glycol, 20.1 parts by weight of trihydroxypropane, 4 parts by weight of monobutyl tin and 6 parts by weight of antioxidant into a reaction kettle, slowly heating the reaction kettle to 150 ℃, and stirring to dissolve materials in the reaction kettle;
b002, slowly adding 2550 parts by weight of terephthalic acid and 355 parts by weight of adipic acid into the reaction kettle, and continuously stirring until the materials in the reaction kettle are uniformly dispersed;
b003, after the materials in the reaction kettle are uniformly dispersed, slowly heating the reaction kettle to 240 ℃, and then keeping the temperature at the top end of the condensing tower below 101 ℃ to distill off water generated in the material reaction;
b004, after water generated in the material reaction is distilled off, continuously keeping the temperature of the reaction kettle at 240 ℃, reducing the temperature of the top end of the condensing tower to 50 ℃, and adding 550 parts by weight of isophthalic acid;
and B005, continuously stirring to ensure that the materials in the reaction kettle react and are clarified, and then starting a vacuum pump to ensure that the materials in the reaction kettle react for 1 hour under negative pressure to obtain the carboxyl-terminated polyester resin.
Has the advantages that:
the invention provides an anti-bending transparent matte high-hardness powder coating and a preparation method thereof, the anti-bending transparent matte high-hardness powder coating does not contain fluorine wax organic components and hard inorganic filler, and a high-branching-degree hydroxyl-terminated polyester resin and closed isocyanate react to form a compact coating with high crosslinking density in the curing process of the powder coating, so that the powder coating has high hardness and scratch resistance; the carboxyl-terminated polyester resin and the epoxy curing agent react to form a coating film with good flexibility, so that the problems that the powder coating is easy to become brittle and poor in impact resistance are solved. In addition, the transparent glass powder is introduced into the powder coating, and the surface of the powder coating generates diffuse reflection by utilizing the incompatibility of other components in the powder coating and the transparent glass powder, so that the glossiness of the powder coating is not too high, a matte effect can be achieved, the powder coating is not easy to show even if the surface of the powder coating has scratches, and the attractiveness of a product is not greatly influenced.
Detailed Description
The invention provides an anti-bending transparent matte high-hardness powder coating and a preparation method thereof, and in order to make the purpose, technical scheme and effect of the invention clearer and clearer, the invention is further described in detail by taking examples as follows. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The invention provides an anti-bending transparent matte high-hardness powder coating which comprises the following components in parts by weight; 130-200 parts of hydroxyl-terminated polyester resin, 130-210 parts of carboxyl-terminated polyester resin, 220-280 parts of blocked isocyanate, 10-25 parts of epoxy curing agent, 10 parts of flatting agent, 5 parts of degassing agent and 340 parts of transparent glass micro powder.
In the curing process of the anti-bending transparent matte high-hardness powder coating, the hydroxyl-terminated polyester resin with high branching degree can react with the closed isocyanate to form a compact coating with high crosslinking density, so that the powder coating can obtain high hardness and scratch resistance; the carboxyl on the carboxyl-terminated polyester resin can react with the epoxy group of the epoxy curing agent to form a coating film with good flexibility, so that the problems of easy brittleness and poor impact resistance of the powder coating are improved; in addition, the transparent glass powder is introduced into the powder coating, and the surface of the powder coating generates diffuse reflection by utilizing the incompatibility of other components in the powder coating and the transparent glass powder, so that the glossiness of the powder coating is not too high, and a matte effect can be achieved.
Furthermore, the ratio of the hydroxyl-terminated polyester resin to the carboxyl-terminated polyester resin is 1: 0.75-1.5 by weight. When the hydroxyl-terminated polyester resin and the carboxyl-terminated polyester resin are used together, if the ratio of the hydroxyl-terminated polyester resin is large, the hardness of the powder coating can be improved, but the flexibility of the powder coating is poor, the adhesion force to the surface of a workpiece is poor, and the powder coating is bright; when the ratio of the carboxyl-terminated polyester resin is large, the flexibility of the powder coating can be improved, but the hardness of the powder coating is low, and the powder coating is bright.
Furthermore, the ratio of the hydroxyl-terminated polyester resin to the blocked isocyanate in parts by weight is 1: 1.5. When the ratio of the hydroxyl-terminated polyester resin is large, the hydroxyl-terminated polyester resin can cause the problem of insufficient reaction due to insufficient use amount of the blocked isocyanate, so that the hardness of the powder coating is not obviously improved; when the ratio of blocked isocyanate is large, the reaction of the hydroxyl-terminated polyester resin is not affected, but the production cost is high,
furthermore, the ratio of the carboxyl-terminated polyester resin to the epoxy curing agent is (8.5-9) to 1.5. When the ratio of the carboxyl-terminated polyester resin is large, the carboxyl-terminated polyester resin can cause the problem of insufficient reaction due to insufficient use amount of the epoxy curing agent, so that the flexibility of the powder coating is not obviously improved; when the proportion of the epoxy curing agent is large, not only is the production cost high, but also the glass transition temperature of a powder coating system is increased, and the flexibility of a powder coating layer is reduced.
The hydroxyl-terminated polyester resin and the carboxyl-terminated polyester resin are reasonably matched and used, when the weight ratio of the hydroxyl-terminated polyester resin to the carboxyl-terminated polyester resin is 1: 0.75-1.5, the weight ratio of the hydroxyl-terminated polyester resin to the blocked isocyanate is 1: 1.5, and the weight ratio of the carboxyl-terminated polyester resin to the epoxy type curing agent is 8.5-9: 1.5, the comprehensive performance of the powder coating is optimal.
Further, the epoxy curing agent is triglycidyl isocyanurate. Compared with other epoxy curing agents, the triglycidyl isocyanurate can improve the ultraviolet resistance of the powder coating, and the triglycidyl isocyanurate has strong reactivity, so that the carboxyl-terminated polyester resin can fully react with the triglycidyl isocyanurate, and the flexibility of the powder coating can be improved.
Specifically, the leveling agent may be the leveling agent GLP-588, and the degassing agent may be the degassing agent BYK-P-104S.
The invention also provides a preparation method of the anti-bending transparent matte high-hardness powder coating, which comprises the following steps:
s001, adding hydroxyl-terminated polyester resin, carboxyl-terminated polyester resin, closed isocyanate, an epoxy curing agent, a flatting agent, a degassing agent and transparent glass micro powder into a mixer for premixing; wherein the premixing time is 5min;
s002, melting and extruding the premixed material in the step S001 through an extruder;
s003, cooling and tabletting the melt-extruded material by using a water-cooled steel belt;
and S004, crushing the flaky material obtained in the step S003 by using a crusher, and sieving to obtain the anti-bending transparent matte high-hardness powder coating.
Furthermore, the temperature of the melting section of the extruder is too high, the raw materials can generate cross-linking curing reaction in the mixing process and can block the extruder on the contrary, and when the temperature of the feed inlet and the melting temperature of the extruder are too low, the mixing effect of the raw materials is not good, the subsequent steps are inconvenient to carry out, and meanwhile, the performance of the powder coating cannot be guaranteed to meet the use requirement. Preferably, in step S002, the temperature of the feed inlet of the extruder is 65 ℃ and the temperature of the melting section is 105 ℃.
Further, in step S004, the particle size of the anti-bending transparent matte high-hardness powder coating is 30 to 50um. When the particle size of the anti-bending transparent matte high-hardness powder coating is within the range, the powder coating is less lost when being sprayed, and meanwhile, the powder coating formed after spraying has good smoothness, so that the powder coating can keep better performance.
Further, in step S001, the method for preparing the hydroxyl-terminated polyester resin comprises the steps of:
step A001, adding 2500 parts by weight of trihydroxypropane and 4 parts by weight of monobutyltin into a reaction kettle connected with a condensing tower, slowly heating the reaction kettle to 150 ℃, and stirring to dissolve the trihydroxypropane;
step A002, slowly adding 1000 parts by weight of terephthalic acid and 1600 parts by weight of isophthalic acid into trihydroxypropane solution, and continuously stirring until the materials in the reaction kettle are uniformly dispersed;
step A003, after the materials in the reaction kettle are uniformly dispersed, slowly heating the reaction kettle to 240 ℃, and then keeping the temperature at the top end of a condensing tower below 101 ℃ to distill off water generated in the material reaction;
and step A004, after water generated in the material reaction is distilled off, continuously keeping the temperature of the reaction kettle at 240 ℃, reducing the temperature of the top end of the condensing tower to 50 ℃, starting a vacuum pump, and carrying out negative pressure reaction on the materials in the reaction kettle for 1 hour to obtain the hydroxyl-terminated polyester resin.
Further, in step S001, the method for preparing the carboxyl group terminated polyester resin comprises the steps of:
b001, adding 1260 parts by weight of neopentyl glycol, 300 parts by weight of ethylene glycol, 20.1 parts by weight of trihydroxypropane, 4 parts by weight of monobutyl tin and 6 parts by weight of antioxidant into a reaction kettle, slowly heating the reaction kettle to 150 ℃, and stirring to dissolve materials in the reaction kettle;
b002, slowly adding 2550 parts by weight of terephthalic acid and 355 parts by weight of adipic acid into the reaction kettle, and continuously stirring until the materials in the reaction kettle are uniformly dispersed;
b003, after the materials in the reaction kettle are uniformly dispersed, slowly heating the reaction kettle to 240 ℃, and then keeping the temperature at the top end of the condensing tower below 101 ℃ to distill off water generated in the material reaction;
b004, after water generated in the material reaction is distilled off, continuously keeping the temperature of the reaction kettle at 240 ℃, reducing the temperature of the top end of the condensing tower to 50 ℃, and adding 550 parts by weight of isophthalic acid;
and B005, continuously stirring to ensure that the materials in the reaction kettle react and are clarified, and then starting a vacuum pump to ensure that the materials in the reaction kettle react for 1 hour under negative pressure to obtain the carboxyl-terminated polyester resin.
The anti-bending transparent matte high-hardness powder coating prepared by the preparation method is sprayed on the surface of a workpiece, and the powder coating is cured to form a powder coating, so that the obtained powder coating has the characteristics of high hardness (the hardness can reach 5H (the pencil hardness is even higher) and scratch resistance, and the powder coating has proper flexibility and strong impact resistance, thereby facilitating the processing of products sprayed with the powder coating, and reducing the appearance damage of the products caused by collision in the use process. In addition, the powder coating formed by the powder coating through curing is a matte transparent coating, can be used for a lighting layer, and cannot influence the color effect of the primer, and the attractiveness of the product cannot be greatly influenced due to scratches on the surface of the powder coating.
To further illustrate the anti-bending transparent matte high-hardness powder coating and the preparation method thereof provided by the invention, the following examples are provided:
example 1
The invention provides an anti-bending transparent matte high-hardness powder coating which comprises the following components in parts by weight; 240 parts of hydroxyl-terminated polyester resin, 360 parts of blocked isocyanate, 10 parts of flatting agent GLP-588, 5 parts of degassing agent BYK-P-104S and 340 parts of transparent glass micropowder.
The invention also provides a preparation method of the anti-bending transparent matte high-hardness powder coating, which comprises the following steps:
step S001, adding hydroxyl-terminated polyester resin, carboxyl-terminated polyester resin, blocked isocyanate, an epoxy curing agent, a flatting agent, a degassing agent and transparent glass micro powder into a mixer for premixing;
s002, melting and extruding the material premixed in the step S001 through an extruder, wherein the temperature of a feed inlet of the extruder is 65 ℃, and the temperature of a melting section is 105 ℃;
s003, cooling and tabletting the melt-extruded material by using a water-cooled steel belt;
and S004, crushing the flaky material obtained in the step S003 by a crusher, and sieving to obtain the anti-bending transparent matte high-hardness powder coating, wherein the particle size of the anti-bending transparent matte high-hardness powder coating is 30-50 um.
Further, in step S001, the method for preparing the hydroxyl-terminated polyester resin comprises the steps of:
step A001, adding 2500 parts by weight of trihydroxypropane and 4 parts by weight of monobutyl tin into a reaction kettle connected with a condensing tower, slowly heating the reaction kettle to 150 ℃, and stirring to dissolve the trihydroxypropane;
step A002, slowly adding 1000 parts by weight of terephthalic acid and 1600 parts by weight of isophthalic acid into a trihydroxypropane solution, and continuously stirring until the materials in the reaction kettle are uniformly dispersed;
step A003, after the materials in the reaction kettle are uniformly dispersed, slowly heating the reaction kettle to 240 ℃, and then keeping the temperature at the top end of a condensing tower below 101 ℃ to distill off water generated in the material reaction;
and step A004, after water generated in the material reaction is distilled off, continuously keeping the temperature of the reaction kettle at 240 ℃, reducing the temperature of the top end of the condensing tower to 50 ℃, starting a vacuum pump, and carrying out negative pressure reaction on the materials in the reaction kettle for 1 hour to obtain the hydroxyl-terminated polyester resin.
Further, in step S001, the method for preparing the carboxyl group terminated polyester resin comprises the steps of:
b001, adding 1260 parts by weight of neopentyl glycol, 300 parts by weight of ethylene glycol, 20.1 parts by weight of trihydroxypropane, 4 parts by weight of monobutyl tin and 6 parts by weight of antioxidant into a reaction kettle, slowly heating the reaction kettle to 150 ℃, and stirring to dissolve materials in the reaction kettle;
b002, slowly adding 2550 parts by weight of terephthalic acid and 355 parts by weight of adipic acid into the reaction kettle, and continuously stirring until the materials in the reaction kettle are uniformly dispersed;
b003, after the materials in the reaction kettle are uniformly dispersed, slowly heating the reaction kettle to 240 ℃, and then keeping the temperature at the top end of the condensing tower below 101 ℃ to distill off water generated in the material reaction;
b004, after water generated in the material reaction is distilled off, continuously keeping the temperature of the reaction kettle at 240 ℃, and adding 550 parts by weight of isophthalic acid after the temperature at the top end of the condensing tower is reduced to 50 ℃;
and B005, continuously stirring to ensure that the materials in the reaction kettle react and are clarified, and then starting a vacuum pump to ensure that the materials in the reaction kettle react for 1 hour under negative pressure to obtain the carboxyl-terminated polyester resin.
Example 2
The invention provides an anti-bending transparent matte high-hardness powder coating which comprises the following components in parts by weight; 200 parts of hydroxyl-terminated polyester resin, 90 parts of carboxyl-terminated polyester resin, 300 parts of blocked isocyanate, 10 parts of triglycidyl isocyanurate, 10 parts of flatting agent GLP-588, 5 parts of degassing agent BYK-P-104S and 340 parts of transparent glass micropowder.
The preparation method of the anti-bending transparent matte high-hardness powder coating is the same as that of the example 1.
Example 3
The invention provides an anti-bending transparent matte high-hardness powder coating which comprises the following components in parts by weight; 180 parts of hydroxyl-terminated polyester resin, 135 parts of carboxyl-terminated polyester resin, 270 parts of blocked isocyanate, 15 parts of triglycidyl isocyanurate, 10 parts of flatting agent GLP-588, 5 parts of degassing agent BYK-P-104S and 340 parts of transparent glass micropowder.
The preparation method of the anti-bending transparent matte high-hardness powder coating is the same as that of the example 1.
Example 4
The invention provides an anti-bending transparent matte high-hardness powder coating which comprises the following components in parts by weight; 150 parts of hydroxyl-terminated polyester resin, 202 parts of carboxyl-terminated polyester resin, 225 parts of blocked isocyanate, 23 parts of triglycidyl isocyanurate, 10 parts of flatting agent GLP-588, 5 parts of degassing agent BYK-P-104S and 340 parts of transparent glass micropowder.
The preparation method of the anti-bending transparent matte high-hardness powder coating is the same as that of the example 1.
Example 5
The invention provides an anti-bending transparent matte high-hardness powder coating which comprises the following components in parts by weight; 100 parts of hydroxyl-terminated polyester resin, 315 parts of carboxyl-terminated polyester resin, 150 parts of blocked isocyanate, 35 parts of triglycidyl isocyanurate, 10 parts of flatting agent GLP-588, 5 parts of degassing agent BYK-P-104S and 340 parts of transparent glass micropowder.
The preparation method of the anti-bending transparent matte high-hardness powder coating is the same as that of the example 1.
Example 6
The invention provides an anti-bending transparent matte high-hardness powder coating which comprises the following components in parts by weight; 40 parts of hydroxyl-terminated polyester resin, 450 parts of carboxyl-terminated polyester resin, 60 parts of blocked isocyanate, 50 parts of triglycidyl isocyanurate, 10 parts of flatting agent GLP-588, 5 parts of degassing agent BYK-P-104S and 340 parts of transparent glass micropowder.
The preparation method of the anti-bending transparent matte high-hardness powder coating is the same as that of the example 1.
The powder coatings prepared in examples 1 to 6 were sprayed on the surface of a workpiece by electrostatic spraying, and then the workpiece coated with the powder coatings was baked in an oven at 200 ℃ for 10min, so that the powder coatings were sufficiently cured to obtain powder coating layers, and the obtained powder coating layers were subjected to performance tests, the test results of which are shown in table 1 below.
In the baking temperature and time of the workpiece, the powder coating layer is discolored and yellowed due to high baking temperature and long baking time, and the decorative effect of the product is further influenced, while the curing process of the powder coating cannot be fully completed due to low baking temperature and short baking time, and the hardness and impact resistance of the powder coating layer are influenced.
TABLE 1 Performance test results for powder coating coatings
In the above table 1, the glossiness (60 ° geometric condition) test of the powder coating is based on the standard GB/T9754-2007 measurement of 20 °, 60 ° and 85 ° specular gloss of the paint film of the color paint and the varnish containing no metallic pigment, the impact resistance test is based on the standard GB/T1732-2020 measurement of impact resistance of the paint film, the adhesion test is based on the standard GB/T9286-2021 compartment test of the color paint and the varnish, the standard of the bending resistance test is based on the GB/T11185-2009 bending test (cone axis) of the color paint and the varnish, and the standard of the pencil hardness test is based on the GB/T26704-2011 pencil.
It should be understood that equivalents and modifications of the technical solution and inventive concept thereof may occur to those skilled in the art, and all such modifications and alterations should fall within the scope of the appended claims.
Claims (10)
1. An anti-bending transparent matte high-hardness powder coating is characterized by comprising the following components in parts by weight; hydroxyl terminated polyester resin 130 ～ 200 parts of carboxyl-terminated polyester resin 130 ～ 210 parts of blocked isocyanate 220 ～ 280 parts of epoxy curing agent 10 ～ 25 parts of flatting agent, 10 parts of degassing agent and 340 parts of transparent glass micro powder.
2. The anti-bending transparent matte high-hardness powder coating according to claim 1, wherein the ratio of the hydroxyl-terminated polyester resin to the carboxyl-terminated polyester resin is 1 to (0.75) in parts by weight ～ 1.5)。
3. The anti-bending transparent matte high-hardness powder coating according to claim 2, wherein the ratio of the hydroxyl-terminated polyester resin to the blocked isocyanate in parts by weight is 1: 1.5.
4. The anti-bending transparent matte high-hardness powder coating according to claim 3, wherein the ratio of the carboxyl-terminated polyester resin to the epoxy curing agent in parts by weight is (8.5) ～ 9)∶1.5。
5. The fold-resistant transparent matte high-hardness powder coating according to claim 1, wherein the epoxy-type curing agent is triglycidyl isocyanurate.
6. A method for preparing the bending-resistant transparent matte high-hardness powder coating according to any one of claims 1 to 5, which comprises the following steps:
s001, adding hydroxyl-terminated polyester resin, carboxyl-terminated polyester resin, closed isocyanate, an epoxy curing agent, a flatting agent, a degassing agent and transparent glass micro powder into a mixer for premixing;
s002, melting and extruding the premixed material in the step S001 through an extruder;
s003, cooling and tabletting the melt-extruded material by using a water-cooled steel belt;
and S004, crushing the flaky material in the step S003 by a crusher, and sieving to obtain the anti-bending transparent matte high-hardness powder coating.
7. The method for preparing the anti-bending transparent matte high-hardness powder coating according to claim 6, wherein in the step S002, the temperature of the feed inlet of the extruder is 65 ℃, and the temperature of the melting section is 105 ℃.
8. The method for preparing the anti-bending transparent matte high-hardness powder coating according to claim 6, wherein in step S004, the particle size of the anti-bending transparent matte high-hardness powder coating is 30 ～ 50um。
9. The method for preparing the anti-bending transparent matte high-hardness powder coating according to claim 6, wherein in the step S001, the method for preparing the hydroxyl-terminated polyester resin comprises the following steps:
step A001, adding 2500 parts by weight of trihydroxypropane and 4 parts by weight of monobutyltin into a reaction kettle connected with a condensing tower, slowly heating the reaction kettle to 150 ℃, and stirring to dissolve the trihydroxypropane;
step A002, slowly adding 1000 parts by weight of terephthalic acid and 1600 parts by weight of isophthalic acid into trihydroxypropane solution, and continuously stirring until the materials in the reaction kettle are uniformly dispersed;
step A003, after the materials in the reaction kettle are uniformly dispersed, slowly heating the reaction kettle to 240 ℃, and then keeping the temperature at the top end of a condensing tower below 101 ℃ to distill off water generated in the material reaction;
and step A004, after water generated in the material reaction is distilled off, continuously maintaining the temperature of the reaction kettle at 240 ℃, reducing the temperature of the top end of the condensing tower to 50 ℃, starting a vacuum pump, and reacting the materials in the reaction kettle for 1 hour under negative pressure to obtain the hydroxyl-terminated polyester resin.
10. The preparation method of the anti-bending transparent matte high-hardness powder coating according to claim 1, wherein in the step S001, the preparation method of the carboxyl-terminated polyester resin comprises the following steps:
b001, adding 1260 parts by weight of neopentyl glycol, 300 parts by weight of ethylene glycol, 20.1 parts by weight of trihydroxypropane, 4 parts by weight of monobutyl tin and 6 parts by weight of antioxidant into a reaction kettle, slowly heating the reaction kettle to 150 ℃, and stirring to dissolve materials in the reaction kettle;
b002, slowly adding 2550 parts by weight of terephthalic acid and 355 parts by weight of adipic acid into the reaction kettle, and continuously stirring until the materials in the reaction kettle are uniformly dispersed;
b003, after the materials in the reaction kettle are uniformly dispersed, slowly heating the reaction kettle to 240 ℃, and then keeping the temperature at the top end of the condensing tower below 101 ℃ to distill off water generated in the material reaction;
b004, after water generated in the material reaction is distilled off, continuously keeping the temperature of the reaction kettle at 240 ℃, and adding 550 parts by weight of isophthalic acid after the temperature at the top end of the condensing tower is reduced to 50 ℃;
and B005, continuously stirring to ensure that the materials in the reaction kettle react and are clarified, and then starting a vacuum pump to ensure that the materials in the reaction kettle react for 1 hour under negative pressure to obtain the carboxyl-terminated polyester resin.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211441179.5A CN115926603A (en) | 2022-11-17 | 2022-11-17 | Anti-bending transparent matte high-hardness powder coating and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211441179.5A CN115926603A (en) | 2022-11-17 | 2022-11-17 | Anti-bending transparent matte high-hardness powder coating and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN115926603A true CN115926603A (en) | 2023-04-07 |
Family
ID=86699973
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202211441179.5A Pending CN115926603A (en) | 2022-11-17 | 2022-11-17 | Anti-bending transparent matte high-hardness powder coating and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN115926603A (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103254745A (en) * | 2013-04-25 | 2013-08-21 | 三棵树涂料股份有限公司 | Super-scratch-resistant unsaturated polyester matte transparent finish paint |
| CN107641451A (en) * | 2017-11-03 | 2018-01-30 | 广西美展化工科技有限公司 | A kind of matt powder coatings and preparation method thereof |
| CN110305576A (en) * | 2019-07-15 | 2019-10-08 | 江西睿智环保科技有限公司 | With anti-graffiti high definition transfer printing wood grain powdery paints, Preparation method and use |
| CN114231135A (en) * | 2021-12-23 | 2022-03-25 | 安徽神剑新材料股份有限公司 | Outdoor mirror powder coating, preparation method thereof and coating formed by same |
-
2022
- 2022-11-17 CN CN202211441179.5A patent/CN115926603A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103254745A (en) * | 2013-04-25 | 2013-08-21 | 三棵树涂料股份有限公司 | Super-scratch-resistant unsaturated polyester matte transparent finish paint |
| CN107641451A (en) * | 2017-11-03 | 2018-01-30 | 广西美展化工科技有限公司 | A kind of matt powder coatings and preparation method thereof |
| CN110305576A (en) * | 2019-07-15 | 2019-10-08 | 江西睿智环保科技有限公司 | With anti-graffiti high definition transfer printing wood grain powdery paints, Preparation method and use |
| CN114231135A (en) * | 2021-12-23 | 2022-03-25 | 安徽神剑新材料股份有限公司 | Outdoor mirror powder coating, preparation method thereof and coating formed by same |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN110922856B (en) | Powder coating with ultrahigh weather-resistant extinction effect | |
| WO2006009219A1 (en) | Thermosetting water-based coating composition and method of forming coating film | |
| GB2421733A (en) | Aqueous amino resin dispersions and thermosetting water-based paint compositions | |
| CN110408311B (en) | Weather-resistant powder coating and preparation method thereof | |
| CN112029081B (en) | Low-temperature curing type metal powder coating, preparation method and polyester resin used in low-temperature curing type metal powder coating | |
| CN108610985B (en) | Low-gloss sheet and molded article thereof | |
| JP4292020B2 (en) | Designable coating film, designable coating film forming method and designable coating composition | |
| CN112920693B (en) | High-wear-resistance vacuum coating hydroxyl acrylic coating and preparation method and application thereof | |
| CN112724801A (en) | Matte powder coating for wheel hub and preparation method thereof | |
| CN115926603A (en) | Anti-bending transparent matte high-hardness powder coating and preparation method thereof | |
| CN111748082A (en) | Special high-performance carboxyl-terminated polyester resin for powder coating and synthesis method thereof | |
| CN115232533B (en) | Super weather-resistant metal powder coating and preparation method thereof | |
| CN110982410A (en) | Electrostatic spraying powder coating and preparation method and application thereof | |
| JP2013215887A (en) | Metallic plastic and method of coating plastic | |
| CN114773940B (en) | Nonpolar polymer material surface treating agent and application thereof | |
| CN112480794A (en) | Mixed extinction powder coating and preparation method thereof | |
| CN116285607A (en) | High-processability coiled material coating composition and preparation method and application thereof | |
| US11203686B2 (en) | Polymer wax powder having a self-repairing function and preparation method thereof | |
| CN113308184A (en) | Bending-resistant weather-resistant powder coating composition for stainless steel and preparation method thereof | |
| CN112724783A (en) | Low-gloss powder coating for hub primer and preparation method thereof | |
| JPH10140073A (en) | Resin composition for coating material | |
| CN110551441A (en) | Super-leveling mirror surface powder coating and preparation method thereof | |
| CN111978527B (en) | High-hardness powder coating with excellent fluorescence performance, preparation method and polyester resin used in preparation method | |
| WO2024082179A1 (en) | Polyester resin for metal powder coating, preparation method therefor, and application thereof | |
| CN110256774B (en) | High-weather-resistance high-gloss white spraying-free ASA material and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20230407 |
|
| RJ01 | Rejection of invention patent application after publication |