CN109354968B - Emulsion and preparation method thereof - Google Patents
Emulsion and preparation method thereof Download PDFInfo
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- CN109354968B CN109354968B CN201811155664.XA CN201811155664A CN109354968B CN 109354968 B CN109354968 B CN 109354968B CN 201811155664 A CN201811155664 A CN 201811155664A CN 109354968 B CN109354968 B CN 109354968B
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- epoxy resin
- emulsion
- humic acid
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- coating
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- 239000000839 emulsion Substances 0.000 title claims abstract description 44
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 238000004945 emulsification Methods 0.000 title description 2
- 239000003822 epoxy resin Substances 0.000 claims abstract description 39
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 39
- QJZYHAIUNVAGQP-UHFFFAOYSA-N 3-nitrobicyclo[2.2.1]hept-5-ene-2,3-dicarboxylic acid Chemical compound C1C2C=CC1C(C(=O)O)C2(C(O)=O)[N+]([O-])=O QJZYHAIUNVAGQP-UHFFFAOYSA-N 0.000 claims abstract description 38
- 239000004021 humic acid Substances 0.000 claims abstract description 38
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- 238000003756 stirring Methods 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 6
- 239000007809 chemical reaction catalyst Substances 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 5
- 238000000614 phase inversion technique Methods 0.000 claims description 5
- 238000001291 vacuum drying Methods 0.000 claims description 5
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims description 2
- 239000003054 catalyst Substances 0.000 claims 1
- 238000000576 coating method Methods 0.000 abstract description 27
- 239000011248 coating agent Substances 0.000 abstract description 16
- 238000005260 corrosion Methods 0.000 abstract description 12
- 230000007797 corrosion Effects 0.000 abstract description 12
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 abstract description 11
- 239000000463 material Substances 0.000 abstract description 8
- 239000003973 paint Substances 0.000 abstract description 6
- 229910021645 metal ion Inorganic materials 0.000 abstract description 4
- 229910000831 Steel Inorganic materials 0.000 abstract description 2
- 239000010959 steel Substances 0.000 abstract description 2
- 230000002035 prolonged effect Effects 0.000 abstract 1
- 238000001179 sorption measurement Methods 0.000 abstract 1
- 239000004593 Epoxy Substances 0.000 description 9
- 239000000758 substrate Substances 0.000 description 6
- 239000000853 adhesive Substances 0.000 description 5
- 230000001070 adhesive effect Effects 0.000 description 5
- 238000000034 method Methods 0.000 description 5
- 150000001875 compounds Chemical class 0.000 description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- 239000002585 base Substances 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
- 238000000746 purification Methods 0.000 description 3
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000000084 colloidal system Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000004132 cross linking Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- -1 iron ions Chemical class 0.000 description 2
- 238000005498 polishing Methods 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical class C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 description 1
- 230000001680 brushing effect Effects 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 239000006071 cream Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000003337 fertilizer Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000005488 sandblasting Methods 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Images
Classifications
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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
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/08—Anti-corrosive paints
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Paints Or Removers (AREA)
- Epoxy Resins (AREA)
Abstract
The invention provides an emulsion and a preparation method thereof, wherein through molecular design, humic acid is grafted to a side chain of epoxy resin, and in the coating process, residual rust on the surface of steel is stable and firmly attached to a base material through the metal ion adsorption chelating capacity of the humic acid, so that the corrosion is prevented from developing continuously; the density of the epoxy resin is increased by grafting the humic acid and the epoxy resin, and the film forming property and the weather resistance of the epoxy resin are enhanced. The emulsion suitable for various base materials provided by the invention has good paint film adhesion, corrosion resistance and weather resistance which are improved compared with common epoxy resin emulsion; the service life of the coating is prolonged, the coating process of the coating is simplified, and most of manpower and material resources are saved.
Description
Technical Field
The invention relates to the technical field of coatings, in particular to an epoxy emulsion for rust-bearing antirust coatings, which can stabilize rust, convert the rust into stable compounds and has good weather resistance.
Background
In recent years, the concept of environmental protection has been advocated, and water-based coatings are attracting more and more attention. Among various aqueous resins, the aqueous epoxy resin has good weather resistance, acid and alkali resistance and small dry film shrinkage, so the aqueous epoxy resin has wide practical application. But as an aqueous matrix, the poor corrosion resistance is still a disadvantage which cannot be avoided in the production and use processes. In the actual use process, the base material metal is required to be polished to be smooth for use, the deep polishing of the base material with a complex shape is extremely difficult, and the corrosion resistance of the base material after use is not good enough. Therefore, the improvement of the complicated using steps and the corrosion resistant effect of the water-based anticorrosive paint in the using process is the central importance of the current work. The resin emulsion is the main film forming matter of the paint and the most abundant component in the paint, so that the performance of the paint is greatly improved by improving the antirust (rust stabilization and rust conversion) capability of the emulsion. Therefore, in order to better adapt to the trend of the large-scale and complicated structure of modern industrial equipment, a high-performance antirust emulsion capable of stably converting the residual rust on the surface of the substrate is urgently needed.
Disclosure of Invention
In order to well solve the technical problems, the application provides the emulsion and the preparation method thereof, wherein the humic acid can be chelated with iron ions to generate a stable compound which is attached to the surface of the matrix, so that the occurrence of 'flash rust' in the coating process of the water-based epoxy emulsion is avoided, the adhesive force between the coating and the matrix is improved, the construction process can be simplified, and the emulsion is widely suitable for buildings with various shapes.
In order to achieve the above purpose, the main technical scheme of the invention is as follows: through molecular design, the humic acid is grafted to a side chain of the epoxy resin to prepare the water-based epoxy emulsion which can be rust-converted and rust-proof and is suitable for buildings in various shapes.
The emulsion is prepared by the following method:
(1) preparation of purified humic acid:
putting humic acid into a three-mouth bottle, adding absolute ethyl alcohol, heating and stirring until the liquid is boiled, filtering, and vacuum drying at 45 ℃ for 12h to obtain purified humic acid.
(2) Preparation of the emulsion:
adding water-based epoxy resin into a three-neck flask, stirring for 15min, adding purified humic acid, adding 98% concentrated sulfuric acid as a reaction catalyst, reacting at 50 ℃ for 3h, slowly adding water, and obtaining emulsion by a phase inversion method.
Wherein the epoxy resin is one or more of E20 epoxy resin, E44 epoxy resin, Ar555 epoxy resin, E51 epoxy resin and H228A epoxy resin.
Wherein the rotating speed of the stirrer is 160r/min-250 r/min.
Wherein, the aqueous epoxy resin and the humic acid are fed according to the ratio of the functionality (-OH: -COOH) of 1-1.2: 4.
The invention has the beneficial effects.
(1) The humic acid is commonly used in fertilizers, has the capability of adsorbing and converting metal ions, can be chelated with iron ions in the coating process by being introduced into the aqueous epoxy emulsion to generate a stable compound and be attached to the surface of a substrate, avoids the occurrence of 'flash rust' in the coating process of the aqueous epoxy emulsion, and simultaneously improves the adhesive force between a coating and the substrate.
(2) The introduction of humic acid in the invention endows the epoxy emulsion with the capability of stabilizing and converting metal ions, so that the coating still has better antirust capability without deeply polishing the substrate in the coating process of the coating, thereby saving a large amount of manpower and material resources, simplifying the coating process and being widely applicable to substrates of various shapes.
(3) The humic acid molecules have a loose net structure and are introduced into the water-based epoxy resin as side chains, so that the crosslinking density of an epoxy resin curing network is increased to a greater extent, the occurrence of a pinhole phenomenon in the drying process of a coating film is reduced to a certain extent, and the performances of corrosion resistance, weather resistance and the like of the coating are improved.
(4) The humic acid has colloid characteristic, and is beneficial to improving the film forming property of the epoxy resin after being introduced into epoxy resin molecules, so that the surface of a paint film is smooth and has no fine pinholes.
(5) The humic acid is a substance extracted from humic substances, and has wide source of raw materials and low price; the emulsion has good stability, and can improve the weather resistance of the emulsion by introducing the side chain of the epoxy resin, thereby prolonging the service life of the coating.
Drawings
Fig. 1 is a reaction mechanism diagram of humic acid grafted epoxy resin.
Fig. 2 is a diagram of the reaction product of humic acid grafted epoxy resin.
Detailed Description
The present invention will be described in further detail with reference to specific examples.
Example 1
(1) Purification of humic acid: taking 30g humic acid into 350ml of three-necked bottle equipped with a stirrer, adding 200ml of absolute ethyl alcohol, placing the three-necked bottle into a water bath kettle for heating, starting the stirrer (the rotating speed is 200 r/min) until the liquid is boiled, taking out and filtering, and carrying out vacuum drying at 45 ℃ for 12h to obtain purified humic acid;
(2) preparation of the emulsion: adding 5g of aqueous epoxy resin into a three-neck flask equipped with a thermometer and a stirrer, stirring for 15min (the rotating speed is 200 r/min), adding 2g of purified humic acid, adding 3 drops of concentrated sulfuric acid as a reaction catalyst, reacting at 50 ℃ for 3h, slowly adding 50ml of water, and obtaining the emulsion by a phase inversion method.
Example 2
(1) Purification of humic acid: taking 30g humic acid into 350ml of three-necked bottle equipped with a stirrer, adding 200ml of absolute ethyl alcohol, placing the three-necked bottle into a water bath kettle for heating, starting the stirrer (the rotating speed is 200 r/min) until the liquid is boiled, taking out and filtering, and carrying out vacuum drying at 45 ℃ for 12h to obtain purified humic acid;
(2) preparation of the emulsion: adding 5g of aqueous epoxy resin into a three-neck flask equipped with a thermometer and a stirrer, stirring for 25min (the rotating speed is 220 r/min), adding 3g of purified humic acid, adding 5 drops of concentrated sulfuric acid as a reaction catalyst, reacting at 50 ℃ for 3h, slowly adding 50ml of water, and obtaining the emulsion by a phase inversion method.
Example 3
(1) Purification of humic acid: taking 30g humic acid into 350ml of three-necked bottle equipped with a stirrer, adding 200ml of absolute ethyl alcohol, placing the three-necked bottle into a water bath kettle for heating, starting the stirrer (the rotating speed is 200 r/min) until the liquid is boiled, taking out and filtering, and carrying out vacuum drying at 45 ℃ for 12h to obtain purified humic acid;
(2) preparation of the emulsion: adding 5g of aqueous epoxy resin into a three-neck flask equipped with a thermometer and a stirrer, stirring for 20min (the rotating speed is 250 r/min), adding 2g of purified humic acid, adding 5 drops of concentrated sulfuric acid as a reaction catalyst, reacting at 50 ℃ for 3h, slowly adding 50ml of water, and obtaining the emulsion by a phase inversion method.
And (5) carrying out comparative test.
To test the performance of the product, unmodified bisphenol A waterborne epoxy resin emulsion and the emulsion prepared according to example 1 of the present application were sprayed onto 5cm × 5cm steel plates (thickness 30 ± 3 μm) without deep sanding and sandblasting, three pieces of each emulsion were sprayed as parallel samples to check the reproducibility of the data, cured at room temperature for three days, and left to test; a rust-preventive emulsion was commercially available as a comparative test. The corrosion resistance and weather resistance of the coating are comprehensively evaluated in the aspects of low-frequency impedance, adhesive force, salt spray test, washing and brushing resistant times, coating appearance and the like when the coating is soaked in 3.5wt% of NaCl for 96 hours, and specific results are shown in the following table.
The performance index comparison table of the six groups of sample sheets shows that: the emulsion of example 1 is superior to the unmodified emulsion in corrosion resistance and adhesion, has improved weather resistance compared with the unmodified emulsion, and is stable without precipitation, cream floating and other phenomena. The modified emulsion reacts with metal ions in the iron rust which is not completely removed to form a stable compound, so that the rust is prevented from continuing to occur, and the adhesive force between the coating and the substrate is improved; the humic acid with a loose net structure is introduced into the epoxy resin side chain, so that the crosslinking density of the epoxy resin is increased, and the colloid characteristic of the humic acid is favorable for forming a film by the epoxy resin; the unmodified emulsion contains partial moisture because of being water-based, and after coating, not only can corrosion be prevented from continuing to a certain extent, but also certain moisture can be provided for corrosion. Meanwhile, compared with the home-made antirust epoxy emulsion of a certain brand, the emulsion has better corrosion resistance and adhesive force than the home-made antirust epoxy emulsion of a certain brand. Therefore, the introduction of humic acid can improve the corrosion resistance of the water-based epoxy emulsion, prolong the service life of the coating, simplify the coating process of the coating and save most of manpower and material resources.
Claims (1)
1. The preparation method of the emulsion is characterized in that the emulsion is prepared by grafting humic acid to a side chain of epoxy resin, and the preparation method comprises the following steps:
(1) preparation of purified humic acid: adding humic acid into ethanol, heating and stirring until the liquid boils, filtering, and vacuum drying the product at 45 deg.C for 12 hr to obtain purified humic acid;
(2) preparation of the emulsion: stirring the aqueous epoxy resin for 15min, adding purified humic acid, stirring uniformly, adding concentrated sulfuric acid as a reaction catalyst, continuously stirring at 50 ℃ for reacting for 3h, slowly adding water, and obtaining emulsion by a phase inversion method;
the epoxy resin is one or more of E20 epoxy resin, E44 epoxy resin, Ar555 epoxy resin, E51 epoxy resin and H228A epoxy resin;
the rotating speed of the stirrer is 160r/min-250 r/min;
the concentration of the concentrated sulfuric acid catalyst is 98 percent;
the water-based epoxy resin and humic acid are mixed according to the ratio of functionality-OH: -COOH ratio of 1-1.2:4, feeding.
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| CN201811155664.XA CN109354968B (en) | 2018-09-30 | 2018-09-30 | Emulsion and preparation method thereof |
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| CN201811155664.XA CN109354968B (en) | 2018-09-30 | 2018-09-30 | Emulsion and preparation method thereof |
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| CN109354968B true CN109354968B (en) | 2021-01-12 |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101240141A (en) * | 2008-03-20 | 2008-08-13 | 焦占付 | Water-based antirust agent |
| CN104496370A (en) * | 2014-12-05 | 2015-04-08 | 江苏格雷特复合材料有限公司 | Preparation method of waterproof material |
| CN105419560A (en) * | 2015-12-12 | 2016-03-23 | 常州大学 | Method for preparing nano-montmorillonite-based anti-corrosion coating |
| CN106147524A (en) * | 2016-07-07 | 2016-11-23 | 合肥市燕美粉末涂料有限公司 | A kind of weather-proof anti-yellowing modification montmorillonite intercalation polymeric modification epoxy resin based powder coating and preparation method thereof |
| CN108587413A (en) * | 2018-05-30 | 2018-09-28 | 安徽润晟建设有限公司 | A kind of exterior wall waterborne epoxy coatings |
-
2018
- 2018-09-30 CN CN201811155664.XA patent/CN109354968B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101240141A (en) * | 2008-03-20 | 2008-08-13 | 焦占付 | Water-based antirust agent |
| CN104496370A (en) * | 2014-12-05 | 2015-04-08 | 江苏格雷特复合材料有限公司 | Preparation method of waterproof material |
| CN105419560A (en) * | 2015-12-12 | 2016-03-23 | 常州大学 | Method for preparing nano-montmorillonite-based anti-corrosion coating |
| CN106147524A (en) * | 2016-07-07 | 2016-11-23 | 合肥市燕美粉末涂料有限公司 | A kind of weather-proof anti-yellowing modification montmorillonite intercalation polymeric modification epoxy resin based powder coating and preparation method thereof |
| CN108587413A (en) * | 2018-05-30 | 2018-09-28 | 安徽润晟建设有限公司 | A kind of exterior wall waterborne epoxy coatings |
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