CN112552800A - Novel single-component water-based FEVE coating resin and preparation method thereof - Google Patents
Novel single-component water-based FEVE coating resin and preparation method thereof Download PDFInfo
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- CN112552800A CN112552800A CN202011302698.4A CN202011302698A CN112552800A CN 112552800 A CN112552800 A CN 112552800A CN 202011302698 A CN202011302698 A CN 202011302698A CN 112552800 A CN112552800 A CN 112552800A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F8/00—Chemical modification by after-treatment
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/14—Polycondensates modified by chemical after-treatment
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Abstract
本发明公开了一种新型单组分水性FEVE涂层树脂及其制备方法，属于FEVE氟碳树脂技术领域，新型单组分水性FEVE涂层树脂，按重量份计，包括：E‑51环氧树脂4～7份，F68聚醚10～14份，PEG4000聚醚10～16份，琥珀酸酐0.6～0.8份，亚麻油酸15～25份，偏苯三酸酐0.5～0.8份，FEVE氟碳树脂5～8份，二甲苯6～8份，丙二醇丁醚8～14份和三乙胺0.8～1.5份；本发明单组分施工，改善了FEVE涂层双组分施工不便的麻烦；本发明经过聚醚的非离子改性，使其具有很好的耐电解质稳定性；本发明涂层树脂的耐候性低于纯的FEVE树脂，高于其他树脂；本发明的涂层树脂具有优异的耐盐雾性(涂层刮板80℃烘30min，再养护7天后测试)，耐盐雾性超过14天，高于同等水性涂料配方的大多数非FEVE类涂层性能。The invention discloses a novel one-component water-based FEVE coating resin and a preparation method thereof, belonging to the technical field of FEVE fluorocarbon resins. The novel one-component water-based FEVE coating resin, in parts by weight, comprises: E-51 epoxy resin Resin 4-7 parts, F68 polyether 10-14 parts, PEG4000 polyether 10-16 parts, succinic anhydride 0.6-0.8 parts, linoleic acid 15-25 parts, trimellitic anhydride 0.5-0.8 parts, FEVE fluorocarbon resin 5-8 parts parts, 6-8 parts of xylene, 8-14 parts of propylene glycol butyl ether and 0.8-1.5 parts of triethylamine; the single-component construction of the invention improves the inconvenient construction of the two-component FEVE coating; The non-ionic modification of the present invention makes it have good resistance to electrolyte stability; the weather resistance of the coating resin of the present invention is lower than that of pure FEVE resin, but higher than that of other resins; the coating resin of the present invention has excellent resistance to salt spray (The coating scraper was baked at 80°C for 30 minutes, and then tested after curing for 7 days), and the salt spray resistance was more than 14 days, which was higher than the performance of most non-FEVE coatings of the same water-based coating formulation.
Description
Technical Field
The invention belongs to the technical field of FEVE fluorocarbon resin, and particularly relates to novel single-component water-based FEVE coating resin and a preparation method thereof.
Background
The FEVE resin coating can be cured at normal temperature and can also be baked and cured at medium and low temperature, and is a leading product of fluorocarbon coatings in China, but the solvent type FEVE coating emits a large amount of VOC gas, the VOC is emitted into the atmosphere to cause photochemical reaction, so that low-altitude ozone is formed to destroy the atmospheric environment, the VOC and suspended particles form secondary aerosol, and the secondary aerosol is harmful to human health.
At present, the FEVE fluorocarbon coating is commonly used for outdoor high-grade protection environment due to excellent weather resistance. However, the conventional FEVE fluorocarbon coating is solvent-based, is constructed by two components, has no environmental protection property and brings inconvenience to construction.
Therefore, the development of a novel single-component aqueous FEVE coating resin which is green, environment-friendly and convenient to construct is of great significance.
Disclosure of Invention
The invention aims to provide a novel single-component waterborne FEVE coating resin and a preparation method thereof, overcomes the defects of the prior art, and provides the novel single-component waterborne FEVE coating resin which is green, environment-friendly and convenient to construct and the preparation method thereof.
The invention provides a novel single-component waterborne FEVE coating resin which comprises the following components in parts by weight: comprises the following components in parts by weight: 4-7 parts of E-51 epoxy resin, 10-14 parts of F68 polyether, 10-16 parts of PEG4000 polyether, 0.6-0.8 part of succinic anhydride, 15-25 parts of linoleic acid, 0.5-0.8 part of trimellitic anhydride, 5-8 parts of FEVE fluorocarbon resin, 6-8 parts of xylene, 8-14 parts of propylene glycol butyl ether and 0.8-1.5 parts of triethylamine.
Furthermore, the FEVE fluorocarbon resin is 50% of the solid content of FEVE fluorocarbon resin in Zhongen chemical industry.
Further, the preparation method of the novel single-component waterborne FEVE coating resin comprises the following steps:
(1) mixing F68 polyether and PEG4000 polyether, and performing vacuum dehydration for 30-60min at the temperature of 110-150 ℃ to obtain a reactant I;
(2) cooling to 45-65 ℃, adding succinic anhydride into the reactant I, slowly heating to 75-90 ℃, and reacting for 1-1.5h under the condition of heat preservation to obtain a reactant II;
(3) adding E-51 epoxy resin into the reactant II, heating to 120-130 ℃, and reacting for 2-4h to obtain a reactant III;
(4) adding FEVE fluorocarbon resin into the reactant III, adding linoleic acid and xylene, heating to 160 ℃ for 130-;
(5) adding an esterification catalyst into the reactant IV, vacuumizing for 0.5-1.5h, and cooling to 180-195 ℃ after detecting that the acid value and the hydroxyl value are qualified to obtain a reactant V;
(6) adding trimellitic anhydride into the reactant V, and reacting for 0.5-1.5h at the temperature of 180-;
(7) cooling to 70-90 ℃, adding triethylamine into the reactant VI, stirring for 20-30min, adding propylene glycol butyl ether, and cooling to 40-50 ℃ to obtain the novel single-component waterborne FEVE coating resin.
Further, the reaction apparatus used in steps (1) to (7) was a three-necked flask with a condenser-water separator. The water separator is a common organic chemical experimental instrument, and the experiment utilizes a constant boiling mixture distillation method, and the water separator is adopted to continuously flow back an organic layer on a water layer generated by reaction into a reaction bottle, so as to remove the generated water.
Further, after the temperature is kept for 20-40min in the step (4), organic matters flow out of the water separator, and then the temperature is continuously increased to 200-230 ℃. When organic matters flow out from the water separator, the reaction is carried out to a saturated state.
Further, the esterification catalyst in the step (5) comprises at least one of titanate and organic tin. The esterification catalyst can be selected adaptively in the prior art depending on the process practice.
Further, in the step (5), the acid value is 25-65mg/KOH, and the hydroxyl value: 20-60 mg/KOH.
The E-51 epoxy resin has water solubility and self-crosslinking property after being modified by polyether and linseed oil.
The FEVE of the invention is modified by linseed oil and trimellitic anhydride to endow single component self-crosslinking property and water solubility, and after the FEVE is modified by mixing with epoxy resin and ions/non-ions, the invention inherits the excellent caking property of the epoxy resin, combines the self weather resistance, simultaneously adds the single component self-crosslinking property, the water solubility and the electrolyte resistance, reduces the trouble of double component blending of solvent type FEVE and greatly facilitates the construction.
The invention has the beneficial effects that:
(1) the coating resin prepared by the invention is constructed in a single component, so that the inconvenience of constructing the FEVE coating in a double component manner is improved;
(2) according to the invention, through nonionic modification of polyether, the coating resin has good electrolyte resistance stability;
(3) the coating resin of the invention has weather resistance lower than that of pure FEVE resin, but higher than that of other resins;
(4) the coating resin has excellent salt fog resistance (tested after a coating scraper is dried for 30min at 80 ℃ and then maintained for 7 days), the salt fog resistance is more than 14 days, and the salt fog resistance is higher than the performance of most non-FEVE coatings of the same water-based paint formula;
(5) the FEVE paint is a solvent type harmful substance paint and is AB bi-component construction, and the FEVE paint in the prior art needs to be prepared in a strict proportion before construction, is expensive, toxic and harmful, and is inconvenient to construct; the performance of the coating is between that of a common non-FEVE coating and a FEVE coating, and the coating is water-based, green and environment-friendly, and has the advantages of convenient single-component construction, high cost performance and wider application range.
Detailed Description
The technical effects of the present invention will be specifically described below by way of examples. It should be noted that the following examples are given solely for the purpose of illustration and are not to be construed as limitations on the scope of the invention, as many insubstantial modifications and variations of the invention may be made by those skilled in the art without departing from the spirit and scope of the invention. The esterification catalyst of the present invention may be titanate and organic tin.
Example 1
The novel one-component waterborne FEVE coating resin of this example comprises, in parts by weight:
the novel single-component waterborne FEVE coating resin provided by the invention is prepared by the following specific steps:
(1) at normal temperature, 10 parts of F68 polyether and 10 parts of PEG4000 polyether are added into a three-necked bottle with a condenser pipe-water separator, and the mixture is vacuumized and dehydrated for 30min at 120 ℃ to remove residual moisture, so as to prepare a reactant I.
(2) And cooling to 50 ℃, adding 0.6 part of succinic anhydride into the reactant I, slowly heating to 80 ℃, and carrying out heat preservation reaction for 1h to obtain a reactant II.
(3) And adding 4 parts of E-51 epoxy resin into the reactant II, heating to 120 ℃, and reacting for 3 hours to obtain a reactant III.
(4) Adding 5 parts of FEVE into the prepared reactant III, adding 15 parts of linoleic acid and 6 parts of dimethylbenzene, heating to 150 ℃, keeping the temperature for 30min, allowing the solvent in the water separator to flow out, continuously heating to 230 ℃, and reacting for 4h to obtain a reactant IV.
(5) And adding an esterification catalyst into the reactant IV, vacuumizing for 1h, and cooling to 190 ℃ to obtain a reactant V after detecting that the acid value is 50mg/KOH and the hydroxyl value is 45mg/KOH are qualified.
(6) 0.5 part of trimellitic anhydride is added into the reactant V, and the reaction is carried out for 1h at 190 ℃ to obtain a reactant VI.
(7) And cooling to 80 ℃, adding 0.8 part of triethylamine into the reactant VI, stirring for 30min, neutralizing to form salt, adding 8 parts of propylene glycol butyl ether, and cooling to 50 ℃ to obtain the novel single-component waterborne FEVE coating resin.
The properties of the novel one-component waterborne FEVE coating resin prepared in this example are as follows:
the characteristics are as follows: single component, convenient construction; the price is lower than 20 yuan/kg;
the salt spray resistance is more than or equal to 13 days;
adhesion: grade 1;
water solubility: the water-soluble emulsion is stable, non-toxic and harmless;
electrolyte resistance characteristics: 0.1% of nitrite salt is added to prevent the nitrite salt from aggregating and precipitating.
Example 2
The novel one-component waterborne FEVE coating resin of this example comprises, in parts by weight:
the novel single-component waterborne FEVE coating resin provided by the invention is prepared by the following specific steps:
(1) at normal temperature, 12 parts of F68 polyether and 13 parts of PEG4000 polyether are added into a three-necked bottle with a condenser pipe-water separator, and the mixture is vacuumized and dehydrated for 60min at 110 ℃ to remove residual moisture, so as to prepare a reactant I.
(2) And cooling to 45 ℃, adding 0.7 part of succinic anhydride into the reactant I, slowly heating to 75 ℃, and carrying out heat preservation reaction for 1.2h to obtain a reactant II.
(3) And adding 5.37 parts of E-51 epoxy resin into the reactant II, heating to 125 ℃, and reacting for 2 hours to obtain a reactant III.
(4) Adding 6.8 parts of FEVE into the prepared reactant III, adding 20.39 parts of linoleic acid and 6 parts of dimethylbenzene, heating to 130 ℃, keeping the temperature for 20min, allowing the solvent in the water separator to flow out, continuously heating to 200 ℃, and reacting for 3h to obtain a reactant IV.
(5) And adding an esterification catalyst into the reactant IV, vacuumizing for 1h, and cooling to 180 ℃ to obtain a reactant V after detecting that the acid value is 25mg/KOH and the hydroxyl value is 20mg/KOH are qualified.
(6) 0.68 part of trimellitic anhydride is added into the reactant V, and the reaction is carried out for 0.5h at 180 ℃ to obtain a reactant VI.
(7) And cooling to 70 ℃, adding 1.22 parts of triethylamine into the reactant VI, stirring for 20min, neutralizing to form salt, adding 12 parts of propylene glycol butyl ether, and cooling to 40 ℃ to obtain the novel single-component aqueous FEVE coating resin.
The properties of the novel one-component waterborne FEVE coating resin prepared in this example are as follows:
the characteristics are as follows: single component, convenient construction; the price is lower than 20 yuan/kg;
the salt spray resistance is more than or equal to 16 days;
adhesion: grade 1;
water solubility: the water-soluble emulsion is stable, non-toxic and harmless;
electrolyte resistance characteristics: 0.1% of nitrite salt is added to prevent the nitrite salt from aggregating and precipitating.
Example 3
The novel one-component waterborne FEVE coating resin of this example comprises, in parts by weight:
the novel single-component waterborne FEVE coating resin provided by the invention is prepared by the following specific steps:
(1) at normal temperature, 14 parts of F68 polyether and 16 parts of PEG4000 polyether are added into a three-necked bottle with a condenser pipe-water separator, and the mixture is vacuumized and dehydrated for 45min at 150 ℃ to remove residual moisture, so as to prepare a reactant I.
(2) And cooling to 65 ℃, adding 0.8 part of succinic anhydride into the reactant I, slowly heating to 90 ℃, and reacting for 1.5 hours under the condition of heat preservation to obtain a reactant II.
(3) And adding 7 parts of E-51 epoxy resin into the reactant II, heating to 130 ℃, and reacting for 4 hours to obtain a reactant III.
(4) Adding 8 parts of FEVE into the prepared reactant III, adding 25 parts of linoleic acid and 8 parts of dimethylbenzene, heating to 160 ℃, keeping the temperature for 40min, allowing the solvent in the water separator to flow out, continuously heating to 215 ℃, and reacting for 3.5h to obtain a reactant IV.
(5) And adding an esterification catalyst into the reactant IV, vacuumizing for 1h, and cooling to 180 ℃ to obtain a reactant V after detecting that the acid value is 25mg/KOH and the hydroxyl value is 20mg/KOH are qualified.
(6) 0.8 part of trimellitic anhydride was added to the reactant V, and the reaction was carried out at 195 ℃ for 1.5 hours to obtain a reactant VI.
(7) And cooling to 90 ℃, adding 1.5 parts of triethylamine into the reactant VI, stirring for 25min, neutralizing to form salt, adding 14 parts of propylene glycol butyl ether, and cooling to 45 ℃ to obtain the novel single-component aqueous FEVE coating resin.
The properties of the novel one-component waterborne FEVE coating resin prepared in this example are as follows:
the characteristics are as follows: single component, convenient construction; the price is lower than 20 yuan/kg;
the salt spray resistance is more than or equal to 21 days;
adhesion: grade 1;
water solubility: the water-soluble emulsion is stable, non-toxic and harmless;
electrolyte resistance characteristics: 0.1% of nitrite salt is added to prevent the nitrite salt from aggregating and precipitating.
Comparative example 1
The coating of the comparative example is a two-component FEVE coating of the prior art.
Two-component FEVE solvent-borne coating (tin-free Wanbo WF-Q211), properties: AB dual component, the construction needs to be allocated according to the proportion strictly, the construction is inconvenient, the price is expensive and is more than 55 yuan/kg.
The coating prepared in this comparative example:
water solubility: water-insoluble, contains a large amount of toxic and harmful organic solvents, and is not environment-friendly.
Electrolyte resistance characteristics: the electrolyte resistance is good.
The above embodiments are merely preferred embodiments of the present invention, which are provided for illustrating the technical solutions of the present invention and not for limiting the same, and it should be understood by those skilled in the art that modifications or equivalent substitutions may be made to the technical solutions of the present invention without departing from the spirit and scope of the present invention, and all of them should be covered by the protection scope of the present invention.
Claims (6)
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Citations (7)
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| US3679618A (en) * | 1969-10-07 | 1972-07-25 | Du Pont | Electrodeposition of fluorocarbon polymers |
| CN101659740A (en) * | 2008-08-28 | 2010-03-03 | 上海涂料有限公司技术中心 | Self-crosslinking sulfonate-base epoxy ester aqueous dispersion and anti-corrosive primer thereof |
| CN104292908A (en) * | 2014-09-04 | 2015-01-21 | 青岛佳尚创意文化有限公司 | Wear resistant paint |
| CN104341877A (en) * | 2013-08-09 | 2015-02-11 | 青岛益群漆业集团有限公司 | Novel fireproof coating |
| CN107540819A (en) * | 2017-09-04 | 2018-01-05 | 山东奔腾漆业股份有限公司 | Dispersible epoxy ester resin and preparation method thereof in a kind of water |
| CN108424521A (en) * | 2018-02-25 | 2018-08-21 | 李嘉顺 | Water-based mono-component epoxy resin latex and preparation method thereof |
| CN111592817A (en) * | 2020-04-14 | 2020-08-28 | 四川轻化工大学 | A kind of fluorocarbon modified water-based alkyd resin coating and preparation method and application thereof |
-
2020
- 2020-11-19 CN CN202011302698.4A patent/CN112552800B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3679618A (en) * | 1969-10-07 | 1972-07-25 | Du Pont | Electrodeposition of fluorocarbon polymers |
| CN101659740A (en) * | 2008-08-28 | 2010-03-03 | 上海涂料有限公司技术中心 | Self-crosslinking sulfonate-base epoxy ester aqueous dispersion and anti-corrosive primer thereof |
| CN104341877A (en) * | 2013-08-09 | 2015-02-11 | 青岛益群漆业集团有限公司 | Novel fireproof coating |
| CN104292908A (en) * | 2014-09-04 | 2015-01-21 | 青岛佳尚创意文化有限公司 | Wear resistant paint |
| CN107540819A (en) * | 2017-09-04 | 2018-01-05 | 山东奔腾漆业股份有限公司 | Dispersible epoxy ester resin and preparation method thereof in a kind of water |
| CN108424521A (en) * | 2018-02-25 | 2018-08-21 | 李嘉顺 | Water-based mono-component epoxy resin latex and preparation method thereof |
| CN111592817A (en) * | 2020-04-14 | 2020-08-28 | 四川轻化工大学 | A kind of fluorocarbon modified water-based alkyd resin coating and preparation method and application thereof |
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