CN102229777A - Hydrophobic olephobic epoxy paint and its preparation and application method - Google Patents
Hydrophobic olephobic epoxy paint and its preparation and application method Download PDFInfo
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Abstract
The invention provides a hydrophobic olephobic epoxy paint and its preparation and application method. The paint is prepared by mixing the following raw materials according to the mass ratio of epoxy paint for color coding: fluorine-silicon copolymer: a mixed solvent: nanometer silica: a curing agent = 1.0 : 0.005-0.12 : 0.5-3.0 : 0-0.30 : 0.01-0.25. An epoxy coating formed by the paint has a microscopic rough structure, overcomes the disadvantage of poor compatibility of an epoxy paint modified by a fluorine-silicon material, and has a water contact angle of 149 degrees and an oil contact angle of 101 degrees, being an epoxy coating with strong hydrophobicity and olephobicity.
Description
Technical field
The invention belongs to low surface energy epoxy coating preparing technical field, be specially a kind of hydrophobic oleophobic epoxy coating and preparation using method thereof.
Technical background
As everyone knows, because epoxy coating has excellent non-corrosibility, chemical-resistant, numerous grounds are had splendid sticking power and good snappiness, in protective coating, occupy dominant position.But, contain in the Resins, epoxy a large amount of hydroxyls (Ye Shoufu. anticorrosive coating summary (on). Shanghai coating, 2000, (3): 25～28), make its surface show stronger absorption property, this has greatly influenced the development and application of high-performance epoxy coating.
In recent years, people have launched the research to new function material and the preparation of exotic materials surface tissue according to the enlightenment to the research of occurring in nature Synthesis of Self-cleaning Bionic Surface.Nowadays, the method for preparing hydrophobic material has a variety of, as: template, etching method, vapour deposition process or the like.The super-hydrophobic self-cleaning Research on surface has more report, but less, the especially domestic research of report of two thin property materials.Give the performance of material surface hydrophobic oleophobic, will greatly widen its range of application.
Summary of the invention
The objective of the invention is to prepare a kind of two thin property epoxy coating.This technology is applied to two opinions of unclogging and readjusting in the epoxy coating, by introducing low surface energy material and nanoparticle, and utilizes the microphase-separated principle, has constructed on the epoxy coating surface to have multiple dimensioned microtexture.The epoxy coat of preparing has strong hydrophobic oleophobic, to the contact angle of water up to 149 °, to the contact angle of oil (whiteruss, as follows) up to 101 °.This method is simple, and cost is low, has extraordinary actual application prospect.
Technical scheme of the present invention is:
A kind of hydrophobic oleophobic epoxy coating, this coating mixes according to the following raw material and the quality proportioning that feeds intake:
Described solidifying agent is trimellitic anhydride (TMA), ethylene glycol bis trimellitic acid 1,2-anhydride ester (TMEG), Tetra hydro Phthalic anhydride (PA) or pyromellitic dianhydride (PMDA);
Described mixed solvent is mixed by dimethylbenzene, propyl carbinol and acetone, and its volume ratio is a dimethylbenzene: propyl carbinol: acetone=3～7: 3～5: 7～10;
Described nano silicon is 10nm～100nm powder;
Described epoxy colored paint is that Tianjin Jin Hai speciality coating is decorated company limited, FXH05-3 epoxy electrostatically conductive oil-tolerant antisepsis finishing paint;
Described fluorine-silicon copolymer thing be fluorinated acrylate-contain vinyltriethoxysilane-styrol copolymer according to following raw material and the quality proportioning that feeds intake through hybrid reaction after breakdown of emulsion, washing and drying form:
Described fluorinated acrylate is perfluor alkyl ethide acrylate, dodecafluorhe-ptylacrylate, methacrylic acid ten difluoro heptyl esters or vinylformic acid hexafluoro butyl ester ester;
The described vinyl silanes that contains is vinyltriethoxysilane, vinyltrimethoxy silane, vinyl triacetyl oxosilane, vinyl three ('beta '-methoxy oxyethyl group) silane, vinyl tributanoximo silane, γ-(methacryloxypropyl) propyl trimethoxy silicane;
The preparation method of described hydrophobic oleophobic epoxy coating prepares according to following steps:
Successively fluorine-silicon copolymer thing, epoxy colored paint, solidifying agent and nano silicon are joined in the reactor according to top material proportioning, and then add mixed solvent, stir, dissolve fully, obtain the epoxy coating of modification up to mixture.
The using method of epoxy coating as described above will be coated in body surface according to the coating of top step gained, be placed on 50 ℃ and solidify 1～5 hour down, be warming up to 120 ℃～200 ℃ again and solidify 1～5 hour, obtain the hydrophobic oleophobic epoxy coat of modification.
The invention has the beneficial effects as follows:
(1) be modified component with fluorinated acrylate-contain vinyltriethoxysilane-styrol copolymer, utilize the good compatibility performance of vinylbenzene segment and epoxy colored paint to be embedded in the epoxy colored paint, and fluorine-containing groups under selected temperature very easily to surface transport, fluorine-containing groups and epoxy colored paint microphase-separated under the condition that these two kinds of competitive power exist, formed the coarse structure of microcosmic, this method is simpler than the method that other makes up coarse structure, and cost is low;
(2) be modified component with the fluorine-silicon copolymer thing, specifically be that fluorinated acrylate-contain vinyltriethoxysilane-styrol copolymer is a modified component, utilize vinylbenzene segment and the good consistency of epoxy colored paint, most of composition of multipolymer can be embedded in the epoxy colored paint like this, thereby has solved the easy problem of separating out from the epoxy colored paint because fluorine-containing groups and epoxy colored paint consistency are bad;
(3) with the nano silicon be filler,, improve its hydrophobic oleophobic at the multiple dimensioned coarse structure of epoxy colored paint surface construction;
(4) select high-temperature curing agent for use; 50 ℃～200 ℃ as the alternating temperature condition of cure; 50 ℃ solidified 2 hours down; during this period of time; the curing speed of solidifying agent is very slow, helps fluorine-containing groups in the multipolymer fully to the epoxy coat surface transport, and epoxy coat just can be covered fully by fluorine-containing groups like this; solidified 1 hour down in 120 ℃～200 ℃ more afterwards, Resins, epoxy is fully solidified.
Beneficial effect (1) has guaranteed that the epoxy coat of structure has certain micro-rough structure; Beneficial effect (2) has guaranteed fluorine-silicon copolymer thing and the good consistency of epoxy coating, thus the bad drawback of consistency when having overcome fluorine silicon materials modified epoxy coating; Beneficial effect (3) has guaranteed the coarse structure on epoxy coat surface, strengthens its hydrophobic oleophobic; (4) guaranteed that fluorine-containing groups moves to the epoxy coat surface fully, thereby given epoxy coat utmost point low surface energy; Thereby make the modified epoxy coating reach 149 °, the contact angle of oil has been reached 101 ° the contact angle of water; Just beneficial effect (1), (3), (4) have guaranteed the strong hydrophobic oleophobic of modified epoxy coating.Under the situation that above three conditions possess simultaneously, the epoxy coat that we make up has reached about 149 ° the contact angle of water, and the contact angle of oil has been reached about 101 °; For example embodiment 1 compares with embodiment 5, under the same terms, adds the nano silicon filler than the coating of not adding the nano silicon filler when the hot setting contact angle of water has been improved 31 °, and the contact angle of oil has been improved 28 °.For example embodiment 5 compares with embodiment 6, under the same terms, adds the fluorine-silicon copolymer thing than the coating of not adding the fluorine-silicon copolymer thing when the hot setting contact angle of water has been improved 38 °, and the contact angle of oil has been improved 49 °.The for example contrast of embodiment 1 and embodiment 5, embodiment 6; Under selected modified component and condition of cure, we have obtained the epoxy coat of strong hydrophobic oleophobic.
Description of drawings
Fig. 1 be among the embodiment 1 epoxy coat to water, to the contact angle test pattern of oil;
Fig. 2 be among the embodiment 5 epoxy coat to water, to the contact angle test pattern of oil;
Fig. 3 be among the embodiment 6 epoxy coat to water, to the contact angle test pattern of oil;
Embodiment
Embodiment 1
One, fluorinated acrylate-the contain preparation and the sign of vinyltriethoxysilane-styrol copolymer:
The sodium lauryl sulphate (SDS), 0.08 gram polyoxyethylene nonylphenol ether (OP-10), 1.5ml C3-Fluoroalcohol, 1.5ml propyl carbinol, 3.0 gram perfluor alkyl ethide acrylate (FA), 0.6 gram vinyltriethoxysilane (VTES), 2.4 gram vinylbenzene (St), the 35 gram distilled water that in the four-hole bottle of 100ml, add 0.04 gram, in 45 ℃ of pre-emulsifications 30 minutes, obtain pre-emulsion.System is warming up to 75 ℃, adds 0.06 gram Diisopropyl azodicarboxylate (AIBN), reacts 4 hours.Reaction finishes back with ethanol or salt solution breakdown of emulsion; Product suction filtration, washing, 50 ℃ of vacuum-dryings obtain perfluor alkyl ethide acrylate-vinyltriethoxysilane-styrol copolymer.
The sign of multipolymer:
3400cm
-1It is the Si-OH peak that vinyl three ethoxy silane hydrolyzates produce; 3062cm
-1Be CH
3Charateristic avsorption band, 2925cm
-1Be CH
2Absorption peak, 3028cm
-1, 1600cm
-1The place is the stretching vibration peak of the c h bond on the phenyl ring, 1739cm
-1The place is the stretching vibration peak of the C=O in the vinylformic acid perfluor alkyl ethide ester, 1212cm
-1, 1150cm
-1The place is the unsymmetrically and the symmetrical peak of C-O key in the ester, 1494cm
-1, 1453cm
-1The place is that general frequency absorption, 1079cm are vibrated in the internal strain of C=C face on the phenyl ring
-1, 1029cm
-1Be the absorption peak of Si-O-Si key, 760cm
-1, 700cm
-1The place has also occurred-CF
2CF
3Absorption peak, have the feature of terpolymer;
Two, the preparation of low surface energy epoxy coating:
(1) takes by weighing above-mentioned perfluor alkyl ethide acrylate-contain vinyltriethoxysilane-styrol copolymer 0.05 gram, solidifying agent TMA 0.1 gram, nano silicon 0.15 restrains to reactor that (the used nano silicon of the present invention is that Shandong hundred million bold and unconstrained type material company limited produces, 10nm～100nm SiO 2 powder), in reactor, add 1.8ml (1.49g) mixed solvent, wherein mixed solvent is by dimethylbenzene, propyl carbinol, acetone is formulated by following volume ratio, dimethylbenzene: propyl carbinol: acetone=7: 3: 7, stir, mixture is dissolved fully;
(2) take by weighing epoxy colored paint (Tianjin Jin Hai speciality coating is decorated company limited, FXH05-3 epoxy electrostatically conductive oil-tolerant antisepsis finishing paint) 1.0 and restrain in reactor, stir, up to dissolving fully;
(3) fully stir, it is mixed, obtain the low surface energy epoxy coating;
Three, the application method of low surface energy epoxy coating:
Mix according to the whole components of top gained, be coated in body surface, be placed on 50 ℃ and solidified 3 hours down, solidified 1 hour down in 150 ℃ again.
Gained modified epoxy coating is 149 ° to the contact angle of water, and the oleophobic angle is 101 ° (seeing accompanying drawing 1), illustrates that the epoxy coat hydrophobic oleophobic is greatly improved.
Product performance testing method of the present invention is as follows: (following examples together)
The matrix surface pre-treatment
Tinplate is all adopted in all substrate test pieces in this experiment, and specimen size is 50mm * 15mm * 0.3mm.Use the 800# sand papering, Ex-all tin layer, iron rust or oxide skin make the metallic surface present even metal gloss, with acetone wiping degrease, dry up, and get final product application after the surface drying.
The brush board requirement
Adopt the method for brushing, come making sheet by standard GB 1727-92 " the general preparation method of paint film ".The model that makes solidifies under the selection temperature, carries out various performance tests then.
Contact angle is measured
About 25 ℃ of room temperatures, adopt sessile drop method to measure the contact angle of coating and water, that is: the position of control syringe needle is in the appropriate position of screen, regulate microsyringe, extracting about 5 μ L water droplets after suction (oil), the de-bubble is added drop-wise on the coating sample, take the shape synoptic diagram of water droplet on coating behind the 20s, calculate contact angle by computer software.Each sample is got 3 different positions arbitrarily and is surveyed its contact angle, gets its mean value.
As shown in Figure 1, the modified epoxy coating is 149 ° to the contact angle of water, and the oleophobic angle is 101 °, illustrates that epoxy coat has excellent hydrophobic oleophobic.
Embodiment 2
Except that the nano silicon consumption was 0.12 gram, other was all with embodiment 1.
Gained modified epoxy coating is 142 ° to the contact angle of water, is 95 ° to the contact angle of oil, illustrates that the epoxy coat hydrophobic oleophobic is greatly improved.
Embodiment 3
Except that the nano silicon consumption was 0.10 gram, other was all with embodiment 1.
Gained modified epoxy coating is 127 ° to the contact angle of water, is 80 ° to the contact angle of oil, illustrates that the epoxy coat hydrophobic oleophobic is improved.
Embodiment 4
Except that the nano silicon consumption was 0.05 gram, other was all with embodiment 1.
Gained modified epoxy coating is 120 ° to the contact angle of water, is 75 ° to the contact angle of oil, illustrates that the epoxy coat hydrophobic oleophobic is greatly improved.
Embodiment 5
Except that nano silicon did not add, other was all with embodiment 1.
Gained modified epoxy coating is 118 ° to the contact angle of water, is 73 ° (seeing accompanying drawing 2) to the contact angle of oil, illustrates that the epoxy coat hydrophobic oleophobic is greatly improved.
Embodiment 6
Outside defluorination silicon polymer and nano silicon did not all add, other was all with embodiment 1.
The gained epoxy coat is 80 ° to the contact angle of water, is 24 ° (seeing accompanying drawing 3) to the contact angle of oil, illustrates that unmodified epoxy coat hydrophobic oleophobic is poor.
Embodiment 7
Defluorination siliceous copolymer consumption is that 0.01g and silicon-dioxide consumption are outside the 0.10g, and other is all with embodiment 1.
Gained modified epoxy coating is 121 ° to the contact angle of water, is 78 ° to the contact angle of oil, illustrates that the epoxy coat hydrophobic oleophobic is greatly improved.
Embodiment 8
Defluorination siliceous copolymer consumption is that 0.03g and silicon-dioxide consumption are outside the 0.05g, and other is all with embodiment 1.
Gained modified epoxy coating is 116 ° to the contact angle of water, is 72 ° to the contact angle of oil, illustrates that the epoxy coat hydrophobic oleophobic is greatly improved.
Embodiment 9
Defluorination siliceous copolymer consumption is that 0.03g and silicon-dioxide consumption are outside the 0.10g, and other is all with embodiment 1.
Gained modified epoxy coating is 138 ° to the contact angle of water, is 87 ° to the contact angle of oil, illustrates that the epoxy coat hydrophobic oleophobic is greatly improved
Embodiment 10
Defluorination siliceous copolymer consumption is that 0.04g and silicon-dioxide consumption are outside the 0.15g, and other is all with embodiment 1.
Gained modified epoxy coating is 143 ° to the contact angle of water, is 91 ° to the contact angle of oil, illustrates that the epoxy coat hydrophobic oleophobic is greatly improved.
Embodiment 11
Desolventizing consumption is outside the 1.2ml (0.99g), and other is all with embodiment 1.
Gained modified epoxy coating is 136 ° to the contact angle of water, is 86 ° to the contact angle of oil, illustrates that the epoxy coat hydrophobic oleophobic is greatly improved.
Embodiment 12
Desolventizing consumption is outside the 2.0ml (1.66g), and other is all with embodiment 1.
Gained modified epoxy coating is 143 ° to the contact angle of water, is 93 ° to the contact angle of oil, illustrates that the epoxy coat hydrophobic oleophobic is greatly improved.
Embodiment 13
Except that hardener dose was 0.05g, other was all with embodiment 1.
Gained modified epoxy coating is 144 ° to the contact angle of water, is 93 ° to the contact angle of oil, illustrates that the epoxy coat hydrophobic oleophobic is greatly improved.
Embodiment 14
Except that hardener dose was 0.20g, other was all with embodiment 1.
Gained modified epoxy coating is 142 ° to the contact angle of water, is 92 ° to the contact angle of oil, illustrates that the epoxy coat hydrophobic oleophobic is greatly improved.
Analyze: (1) embodiment 5 is that with the difference of embodiment 6 embodiment 5 has added the fluorine-silicon copolymer thing; And do not add fluorine-silicon copolymer thing and nano silicon among the embodiment 6.The result is, the coating that embodiment 5 obtains is 118 ° to the contact angle of water, is 73 ° to the contact angle of oil; And the contact angle of 6 pairs of water of embodiment only is 80 °, is 24 ° to the contact angle of oil, illustrates that the raising that filler fluorine-silicon copolymer thing is introduced the epoxy coat hydrophobic oleophobic has significant effect.
(2) embodiment 5 is that with the difference of embodiment 1 embodiment 1 has added nano silicon; And do not add the nano silicon filler among the embodiment 5.The result is: the coating that embodiment 1 obtains is 149 ° to the contact angle of water, is 101 ° to the contact angle of oil; And the contact angle of 5 pairs of water of embodiment only is 118 °, is 73 ° to the contact angle of oil, and the introducing that filler nanometer silicon-dioxide is described has significant effect to the raising of epoxy coat hydrophobic oleophobic.
(3) embodiment 6 is that with the difference of embodiment 1 embodiment 1 has added nano silicon and fluorine-silicon copolymer thing; And do not add above-mentioned substance among the embodiment 6.The result is, the coating that embodiment 1 obtains is 149 ° to the contact angle of water, is 101 ° to the contact angle of oil; And the contact angle of 6 pairs of water of embodiment only is 80 °, is 24 ° to the contact angle of oil, and the introducing that filler fluorine-silicon copolymer thing and nano silicon be described has significant effect to the raising of epoxy coat hydrophobic oleophobic.
Claims (6)
1. hydrophobic oleophobic epoxy coating is characterized by this coating and mixes according to the following raw material and the quality proportioning that feeds intake:
Described solidifying agent is trimellitic anhydride (TMA), ethylene glycol bis trimellitic acid 1,2-anhydride ester (TMEG), Tetra hydro Phthalic anhydride (PA) or pyromellitic dianhydride (PMDA);
Described mixed solvent is mixed by dimethylbenzene, propyl carbinol and acetone, and its volume ratio is a dimethylbenzene: propyl carbinol: acetone=3～7: 3～5: 7～10;
Described nano silicon is 10nm～100nm powder;
Described epoxy colored paint is that Tianjin Jin Hai speciality coating is decorated company limited, FXH05-3 epoxy electrostatically conductive oil-tolerant antisepsis finishing paint.
2. hydrophobic oleophobic epoxy coating according to claim 1, it is characterized by described fluorine-silicon copolymer thing and be fluorinated acrylate-contain vinyltriethoxysilane-styrol copolymer, according to following raw material and the quality proportioning that feeds intake through hybrid reaction after breakdown of emulsion, washing and drying form:
3. as hydrophobic oleophobic epoxy coating as described in the claim 2, it is characterized by described fluorinated acrylate is perfluor alkyl ethide acrylate, dodecafluorhe-ptylacrylate, methacrylic acid ten difluoro heptyl esters or vinylformic acid hexafluoro butyl ester ester;
4. as hydrophobic oleophobic epoxy coating as described in the claim 2, it is characterized by the described vinyl silanes that contains is vinyltriethoxysilane, vinyltrimethoxy silane, vinyl triacetyl oxosilane, vinyl three ('beta '-methoxy oxyethyl group) silane, vinyl tributanoximo silane or γ-(methacryloxypropyl) propyl trimethoxy silicane.
5. the preparation method of hydrophobic oleophobic epoxy coating as claimed in claim 1 is characterized by according to following steps and prepares:
Successively fluorine-silicon copolymer thing, epoxy colored paint, solidifying agent and nano silicon are joined in the reactor according to top material proportioning, and then add mixed solvent, stir, dissolve fully, obtain the epoxy coating of modification up to mixture.
6. the using method of hydrophobic oleophobic epoxy coating as claimed in claim 1, it is characterized by: the coating of gained is coated in body surface, be placed on 50 ℃ and solidified 1～5 hour down, be warming up to 120 ℃～200 ℃ again and solidified 1～5 hour, obtain the hydrophobic oleophobic epoxy coat of modification.
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| CN102660871A (en) * | 2012-04-13 | 2012-09-12 | 江苏嘉业氟材料科技有限公司 | Fluorine containing water repellent oil repellent composition and its preparation method |
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| CN115948118B (en) * | 2021-10-08 | 2023-10-27 | 四川大学 | Environment-adaptive aqueous super-amphiphobic flame-retardant coating, preparation method and coating |
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