CN114316744A - Polyethylene terephthalate crystal-reinforced epoxy resin coating and preparation method thereof - Google Patents
Polyethylene terephthalate crystal-reinforced epoxy resin coating and preparation method thereof Download PDFInfo
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- CN114316744A CN114316744A CN202111680767.XA CN202111680767A CN114316744A CN 114316744 A CN114316744 A CN 114316744A CN 202111680767 A CN202111680767 A CN 202111680767A CN 114316744 A CN114316744 A CN 114316744A
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- 239000003822 epoxy resin Substances 0.000 title claims abstract description 81
- 229920000647 polyepoxide Polymers 0.000 title claims abstract description 81
- 238000000576 coating method Methods 0.000 title claims abstract description 53
- 239000011248 coating agent Substances 0.000 title claims abstract description 52
- -1 Polyethylene terephthalate Polymers 0.000 title claims description 39
- 229920000139 polyethylene terephthalate Polymers 0.000 title claims description 36
- 239000005020 polyethylene terephthalate Substances 0.000 title claims description 36
- 238000002360 preparation method Methods 0.000 title abstract description 12
- 239000002202 Polyethylene glycol Substances 0.000 claims abstract description 25
- 229920001223 polyethylene glycol Polymers 0.000 claims abstract description 25
- KKEYFWRCBNTPAC-UHFFFAOYSA-L terephthalate(2-) Chemical compound [O-]C(=O)C1=CC=C(C([O-])=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-L 0.000 claims abstract description 25
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 22
- BYEAHWXPCBROCE-UHFFFAOYSA-N 1,1,1,3,3,3-hexafluoropropan-2-ol Chemical compound FC(F)(F)C(O)C(F)(F)F BYEAHWXPCBROCE-UHFFFAOYSA-N 0.000 claims abstract description 19
- 238000001723 curing Methods 0.000 claims abstract description 15
- 238000003756 stirring Methods 0.000 claims abstract description 13
- 239000002518 antifoaming agent Substances 0.000 claims abstract description 11
- 238000002425 crystallisation Methods 0.000 claims abstract description 10
- 230000008025 crystallization Effects 0.000 claims abstract description 10
- 238000002156 mixing Methods 0.000 claims abstract description 8
- 239000002994 raw material Substances 0.000 claims abstract description 3
- 238000007789 sealing Methods 0.000 claims description 11
- 239000000463 material Substances 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 8
- 239000013078 crystal Substances 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 5
- 239000002904 solvent Substances 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 239000002184 metal Substances 0.000 claims description 4
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 2
- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 2
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 claims description 2
- 238000002844 melting Methods 0.000 claims description 2
- 230000008018 melting Effects 0.000 claims description 2
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 2
- 229920006122 polyamide resin Polymers 0.000 claims description 2
- 229920000728 polyester Polymers 0.000 claims description 2
- 229920000570 polyether Polymers 0.000 claims description 2
- 230000007797 corrosion Effects 0.000 abstract description 12
- 238000005260 corrosion Methods 0.000 abstract description 12
- 238000013329 compounding Methods 0.000 abstract 2
- 239000005028 tinplate Substances 0.000 description 9
- 239000003973 paint Substances 0.000 description 5
- 239000011521 glass Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 239000012815 thermoplastic material Substances 0.000 description 4
- 230000004888 barrier function Effects 0.000 description 3
- 238000004321 preservation Methods 0.000 description 3
- 229920005989 resin Polymers 0.000 description 3
- 239000011347 resin Substances 0.000 description 3
- 229920005992 thermoplastic resin Polymers 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000005484 gravity Effects 0.000 description 2
- 239000002861 polymer material Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 229920001187 thermosetting polymer Polymers 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- APWRLAZEMYLHKZ-UHFFFAOYSA-N 2-amino-5,6-dimethyl-1h-pyrimidin-4-one Chemical compound CC=1NC(N)=NC(=O)C=1C APWRLAZEMYLHKZ-UHFFFAOYSA-N 0.000 description 1
- 241001391944 Commicarpus scandens Species 0.000 description 1
- 239000004952 Polyamide Substances 0.000 description 1
- 239000004697 Polyetherimide Substances 0.000 description 1
- 239000004642 Polyimide Substances 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000010485 coping Effects 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229920006334 epoxy coating Polymers 0.000 description 1
- 125000003700 epoxy group Chemical group 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 229920000578 graft copolymer Polymers 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920002492 poly(sulfone) Polymers 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- 229920001610 polycaprolactone Polymers 0.000 description 1
- 239000004632 polycaprolactone Substances 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- 229920001601 polyetherimide Polymers 0.000 description 1
- 229920001721 polyimide Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 229920001169 thermoplastic Polymers 0.000 description 1
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Abstract
The invention discloses an epoxy resin coating with enhanced polyethylene glycol terephthalate crystallization and a preparation method thereof, wherein the coating comprises the following raw materials in percentage by mass: 36.5 to 39.5 percent of epoxy resin; 0.5 to 5 percent of polyethylene glycol terephthalate; 40% of hexafluoroisopropanol; 18.3 to 19.8 percent of curing agent; 0.1% of leveling agent; 0.1 percent of defoaming agent. The coating is prepared according to the steps of dissolving, compounding, stirring, blending, curing, baking and the like, and the mechanical property and the corrosion resistance of the cured epoxy resin are improved through the crystallization behavior of the polyethylene glycol terephthalate in the coating, and the optimal compounding ratio is obtained.
Description
Technical Field
The invention relates to a high polymer material and a preparation method thereof, in particular to an epoxy resin coating with enhanced polyethylene terephthalate crystallization and a preparation method thereof.
Background
The coating is the most economic and effective means for dealing with metal corrosion at present, and the most common and efficient coating used in the anticorrosion coating is mainly a thermosetting resin material. Epoxy resin is a thermosetting resin, and polar groups with extremely strong activity, such as epoxy groups and hydroxyl groups, exist in the curing process of the epoxy resin, so that the epoxy resin gives extremely high adhesion, and a cured product of the epoxy resin has high strength and bonding performance and is widely applied to coatings and adhesives. However, as a bulk type polycondensation polymer material, an epoxy resin is apt to undergo further improvement of the degree of curing and aging during use, and a crosslinked network having a high density is formed after curing, and this network structure makes the paint film have a high cohesive force, the paint film has a low modulus and becomes brittle, and is difficult to deform by an external force, and is easy to break and poor in impact resistance. Therefore, modifying the epoxy resin without changing the properties of the epoxy resin itself to obtain more properties of the epoxy resin has become a research focus for coping with different use environments and more professional fields.
The polyethylene terephthalate is a milky white or light yellow highly crystalline polymer, has smooth and glossy surface, and has excellent mechanical properties and chemical stability. Meanwhile, the polyethylene terephthalate has higher barrier property to oxygen, water vapor, carbon dioxide and the like, so the performance of the epoxy resin is further improved by blending the polyethylene terephthalate to the epoxy resin. For example, Kevser Bal or the like glycolyzes a waste polyethylene terephthalate plastic bottle at 180 to 190 ℃ and extracts the reaction products with boiling water, and then synthesizes the products into polyethylene terephthalate-based epoxy resin. The chemical and physical properties of a paint film of the epoxy resin paint containing the waste polyethylene terephthalate are experimentally measured, and the hardness, dryness and chemical properties of the paint film are improved, and the excellent adhesive force, cleaning resistance and water resistance of the epoxy resin are maintained. "CN 104559063A" discloses "a high-toughness low-shrinkage epoxy resin composition, an insulating member and a preparation method thereof", which utilizes thermoplastic resins such as polyamide, maleic anhydride copolymer, maleic anhydride graft polymer and the like to modify epoxy resin, and has the characteristics of high impact strength, no shrinkage and the like. "CN 109111167A" discloses "a stretch-resistant cement-based permeable crystalline waterproof material", which introduces flexible long-chain structure into epoxy coating to improve the strength and stability of waterproof coating. "CN 104371275A" discloses "an epoxy resin composite material synergistically modified by nano-cellulose-thermoplastic resin and a preparation method thereof", which modifies epoxy resin by environment-friendly and green nano-cellulose and thermoplastic resin polyimide, polyetherimide, polysulfone and polycaprolactone together, improves interface bonding force, and realizes synergistic reinforcement and toughening of the epoxy resin. "CN 112831254A" discloses "a metal antirust coating and a preparation method thereof", which combines and promotes polyurethane modified epoxy resin and polypropylene resin by dipropyl adipate to form a mutual transmission network structure, thereby improving the binding force and the corrosion resistance of the coating.
Disclosure of Invention
The purpose of the invention is as follows: the invention aims to provide an epoxy resin coating with enhanced crystallization of polyethylene terephthalate, which has better corrosion resistance and mechanical properties.
Another object of the present invention is to provide a method for preparing the crystal-reinforced polyethylene terephthalate epoxy resin coating having better corrosion resistance and mechanical properties.
The technical scheme is as follows: the invention provides a polyethylene terephthalate crystal reinforced epoxy resin coating, which comprises the following raw materials in percentage by mass: 36.5 to 39.5 percent of epoxy resin; 0.5 to 5 percent of polyethylene glycol terephthalate; 40% of hexafluoroisopropanol; 18.3 to 19.8 percent of curing agent; 0.1% of leveling agent; 0.1 percent of defoaming agent.
Further, the epoxy resin is E-51 epoxy resin. The polyethylene terephthalate has a number-average molecular weight Mn of 2X 104 g/mol. The curing agent is a polyamide resin. The leveling agent is polyether polyester modified organic siloxane. The defoaming agent is polydimethylsiloxane.
The preparation method of the polyethylene terephthalate crystal reinforced epoxy resin coating comprises the following steps: melting polyethylene glycol terephthalate, then placing the melted polyethylene glycol terephthalate into water to cool and reduce the crystallinity, then adding hexafluoroisopropanol solvent, sealing and standing until the melted polyethylene glycol terephthalate is completely dissolved, adding a proper amount of epoxy resin into a polyethylene glycol terephthalate/hexafluoroisopropanol system, stirring the polyethylene glycol terephthalate/hexafluoroisopropanol/epoxy resin system at normal temperature until the system is in a uniform, colorless and transparent state, then adding a curing agent into a blending system, dropwise adding a flatting agent and an antifoaming agent, fully stirring, sealing and standing, then coating the blend on a metal sheet, baking, and then carrying out isothermal crystallization treatment on the coating.
Aiming at the defects that the prior epoxy resin is poor in impact resistance after being cured, poor in toughness, easy to generate cracks after the coating is damaged due to large brittleness and promote substrate corrosion and the like, the epoxy resin and the crystallizable thermoplastic material are blended, so that the mechanical property of the epoxy resin is improved, the generation of the cracks is reduced, and the corrosion resistance of the epoxy resin is improved by utilizing the excellent barrier property of the crystallizable thermoplastic material. The invention aims to overcome the defects that the prior epoxy resin has poor impact resistance after being cured, has poor toughness, is easy to generate cracks after the coating is damaged due to large brittleness, promotes substrate corrosion and the like, and blend the epoxy resin and the crystallizable thermoplastic material, thereby improving the mechanical property of the epoxy resin and reducing the generation of the cracks on the one hand, and improving the corrosion resistance of the epoxy resin by utilizing the excellent barrier property of the crystallizable thermoplastic material on the other hand. The polyethylene terephthalate which is a thermoplastic polymer with a crystal structure is used for modifying the epoxy resin, so that the corrosion resistance of the epoxy resin is effectively improved. As the mass fraction and specific gravity of the polyethylene terephthalate are increased under the compound system, as shown in figure 1, the impedance of the epoxy resin coating enhanced by the polyethylene terephthalate crystallization shows a continuously increasing process, and the corrosion resistance is effectively enhanced when the mass of the polyethylene terephthalate is 5%.
Has the advantages that: the invention can better improve the mechanical property and corrosion resistance of the cured epoxy resin while maintaining the excellent performance of the epoxy resin coating. The invention finds out a reasonable proportion of the compound components through experiments and obtains better performance parameters.
Drawings
FIG. 1 shows the situation that the specific gravity of the compounded system is increased along with the mass fraction of the polyethylene terephthalate.
Detailed Description
Example 1:
the crystal-reinforced epoxy resin coating without polyethylene terephthalate is prepared from the following materials in percentage by mass:
placing the epoxy resin in an oven, carrying out heat preservation treatment at 60 ℃ for 20min, respectively taking a proper amount of epoxy resin to dissolve the epoxy resin with hexafluoroisopropanol after the viscosity is reduced, and manually stirring the epoxy resin for 5min at normal temperature until the system is in a uniform, colorless and transparent state. Adding an epoxy resin curing agent, a flatting agent and a defoaming agent into the blending system, fully stirring by using a glass rod, sealing and standing for 10min, coating the blend on a tinplate, placing the tinplate in an oven at 100 ℃ and baking for 2h, and taking out the tinplate. The impedance of the coating without the polyethylene terephthalate epoxy resin is about 4X 103Ω。
Example 2:
the polyethylene glycol terephthalate crystal reinforced epoxy resin coating is prepared from the following materials in percentage by mass:
adding melt-quenched polyethylene glycol terephthalate into hexafluoroisopropanol solvent, sealing and standing for 2h to completely dissolve, then placing the epoxy resin in an oven, and keeping the temperature at 60 DEG CTreating for 20min, and respectively adding proper amount of epoxy resin into a polyethylene terephthalate/hexafluoroisopropanol system after the viscosity is reduced. And (3) manually stirring the polyethylene terephthalate/hexafluoroisopropanol/epoxy resin system for 5min at normal temperature until the system is in a uniform, colorless and transparent state. Adding an epoxy resin curing agent, a flatting agent and a defoaming agent into the blending system, fully stirring by using a glass rod, sealing and standing for 10min, coating the blend on a tinplate, placing the tinplate in a 100 ℃ oven for baking for 2h, and then carrying out 120 ℃ isothermal crystallization treatment on the coating for 1h to finish the preparation of the coating. The surface of the coating is flat and smooth, and has network-shaped bulges which are light white and transparent. The impedance of the coated sample with 0.5% polyethylene terephthalate was about 1X 104Ω。
Example 3:
the polyethylene glycol terephthalate crystal reinforced epoxy resin coating is prepared from the following materials in percentage by mass:
adding the melt-quenched polyethylene glycol terephthalate into a hexafluoroisopropanol solvent, sealing and standing for 2h to completely dissolve the polyethylene glycol terephthalate, then placing the epoxy resin into an oven, carrying out heat preservation treatment at 60 ℃ for 20min, and respectively adding a proper amount of the epoxy resin into a polyethylene glycol terephthalate/hexafluoroisopropanol system after the viscosity is reduced. And (3) manually stirring the polyethylene terephthalate/hexafluoroisopropanol/epoxy resin system for 5min at normal temperature until the system is in a uniform, colorless and transparent state. Adding an epoxy resin curing agent, a flatting agent and a defoaming agent into the blending system, fully stirring by using a glass rod, sealing and standing for 10min, coating the blend on a tinplate, placing the tinplate in a 100 ℃ oven for baking for 2h, and then carrying out 120 ℃ isothermal crystallization treatment on the coating for 1h to finish the preparation of the coating. The surface of the coating is relatively flat, and obvious network-shaped tissues appear on the part of the coating, and the coating is light white and transparent. The impedance of the coated sample having a polyethylene terephthalate content of 2.5% was about 1.5X 104Ω。
Example 4:
the polyethylene glycol terephthalate crystal reinforced epoxy resin coating is prepared from the following materials in percentage by mass:
adding the melt-quenched polyethylene glycol terephthalate into a hexafluoroisopropanol solvent, sealing and standing for 2h to completely dissolve the polyethylene glycol terephthalate, then placing the epoxy resin into an oven, carrying out heat preservation treatment at 60 ℃ for 20min, and respectively adding a proper amount of the epoxy resin into a polyethylene glycol terephthalate/hexafluoroisopropanol system after the viscosity is reduced. And (3) manually stirring the polyethylene terephthalate/hexafluoroisopropanol/epoxy resin system for 5min at normal temperature until the system is in a uniform, colorless and transparent state. Adding an epoxy resin curing agent, a flatting agent and a defoaming agent into the blending system, fully stirring by using a glass rod, sealing and standing for 10min, coating the blend on a tinplate, placing the tinplate in a 100 ℃ oven for baking for 2h, and then carrying out 120 ℃ isothermal crystallization treatment on the coating for 1h to finish the preparation of the coating. The coating has rough surface, is distributed with granular substances, presents grey white and has lower transparency. The impedance of the coated sample having a polyethylene terephthalate content of 2.5% was about 1.5X 105Ω。
Claims (7)
1. The polyethylene terephthalate crystal reinforced epoxy resin coating is characterized in that: the material comprises the following raw materials in percentage by mass: 36.5 to 39.5 percent of epoxy resin; 0.5 to 5 percent of polyethylene glycol terephthalate; 40% of hexafluoroisopropanol; 18.3 to 19.8 percent of curing agent; 0.1% of leveling agent; 0.1 percent of defoaming agent.
2. The polyethylene terephthalate crystal-reinforced epoxy resin coating according to claim 1, characterized in that: the epoxy resin is E-51 epoxy resin.
3. The polyethylene terephthalate crystal-reinforced epoxy resin coating according to claim 1, characterized in that: the polyethylene terephthalate has a number-average molecular weight Mn of 2X 104 g/mol.
4. The polyethylene terephthalate crystal-reinforced epoxy resin coating according to claim 1, characterized in that: the curing agent is a polyamide resin.
5. The polyethylene terephthalate crystal-reinforced epoxy resin coating according to claim 1, characterized in that: the leveling agent is polyether polyester modified organic siloxane.
6. The polyethylene terephthalate crystal-reinforced epoxy resin coating according to claim 1, characterized in that: the defoaming agent is polydimethylsiloxane.
7. The process for producing a polyethylene terephthalate crystal-reinforced epoxy resin coating material according to any one of claims 1 to 6, characterized in that: the method comprises the following steps: melting polyethylene glycol terephthalate, then placing the melted polyethylene glycol terephthalate into water to cool and reduce the crystallinity, then adding hexafluoroisopropanol solvent, sealing and standing until the melted polyethylene glycol terephthalate is completely dissolved, adding a proper amount of epoxy resin into a polyethylene glycol terephthalate/hexafluoroisopropanol system, stirring the polyethylene glycol terephthalate/hexafluoroisopropanol/epoxy resin system at normal temperature until the system is in a uniform, colorless and transparent state, then adding a curing agent into a blending system, dropwise adding a flatting agent and an antifoaming agent, fully stirring, sealing and standing, then coating the blend on a metal sheet, baking, and then carrying out isothermal crystallization treatment on the coating.
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| CN202111680767.XA CN114316744A (en) | 2021-12-31 | 2021-12-31 | Polyethylene terephthalate crystal-reinforced epoxy resin coating and preparation method thereof |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20040197571A1 (en) * | 2003-04-03 | 2004-10-07 | Yuji Hiroshige | Thermosetting composition, and sealing article and sealing structure using the same |
| US20070093583A1 (en) * | 2003-10-28 | 2007-04-26 | Asahi Kasei Chemicals Corporation | Polytrimethylene terephthalate reinforced resin composition |
| CN109554069A (en) * | 2018-11-15 | 2019-04-02 | 江苏科技大学 | A kind of epoxy coating and preparation method thereof of nylon crystallization enhancing |
| CN112409571A (en) * | 2020-10-30 | 2021-02-26 | 青岛爱尔家佳新材料股份有限公司 | Preparation method of hyperbranched epoxy resin, damping constrained layer coating and preparation method |
| CN112778697A (en) * | 2019-11-07 | 2021-05-11 | 万华化学集团股份有限公司 | Crystalline thermoplastic epoxy resin condensate and preparation method thereof |
-
2021
- 2021-12-31 CN CN202111680767.XA patent/CN114316744A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20040197571A1 (en) * | 2003-04-03 | 2004-10-07 | Yuji Hiroshige | Thermosetting composition, and sealing article and sealing structure using the same |
| US20070093583A1 (en) * | 2003-10-28 | 2007-04-26 | Asahi Kasei Chemicals Corporation | Polytrimethylene terephthalate reinforced resin composition |
| CN109554069A (en) * | 2018-11-15 | 2019-04-02 | 江苏科技大学 | A kind of epoxy coating and preparation method thereof of nylon crystallization enhancing |
| CN112778697A (en) * | 2019-11-07 | 2021-05-11 | 万华化学集团股份有限公司 | Crystalline thermoplastic epoxy resin condensate and preparation method thereof |
| CN112409571A (en) * | 2020-10-30 | 2021-02-26 | 青岛爱尔家佳新材料股份有限公司 | Preparation method of hyperbranched epoxy resin, damping constrained layer coating and preparation method |
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