CN101857765B - Epoxy resin coating and preparation method thereof - Google Patents
Epoxy resin coating and preparation method thereof Download PDFInfo
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- CN101857765B CN101857765B CN2010102143020A CN201010214302A CN101857765B CN 101857765 B CN101857765 B CN 101857765B CN 2010102143020 A CN2010102143020 A CN 2010102143020A CN 201010214302 A CN201010214302 A CN 201010214302A CN 101857765 B CN101857765 B CN 101857765B
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Abstract
The invention provides an epoxy resin coating, which consists of resin components and curing agent components; the resin components include 25 to 40 percent by weight of epoxy resin with the epoxy equivalent weight of 235 to 265, 3 to 6.5 percent by weight of epoxy resin with the epoxy equivalent weight of 170 to 195, 0.2 to 0.7 percent by weight of dispersant, 1 to 2 percent by weight of levelling agent, 5 to 12 percent by weight of diluent and 50 to 65 percent by weight of filling; the curing agent components include 18 to 26 percent by weight of phenolic aldehyde amine modified curing agent, 52 to 66 percent by weight of cashew nut oil modified phenolic aldehyde amine curing agent and 10 to 25 percent by weight of dimethylbenzene; and the weight ratio of the resin components to the curing agent components is 6 to 7:1. The invention also provides a method for preparing the epoxy resin coating. The provided epoxy resin coating is non-toxic, and can be used on conduits and equipment which are directly contacted with food.
Description
Technical field
The present invention relates to paint field, particularly a kind of epoxy coating and preparation method thereof.
Background technology
Coating is a kind of Chemicals that contain pigment or do not contain pigment, process with resin and wet goods.Again can dry and hard film forming on the body surface with applying coating, the surface of coated article body and surrounding medium are separated, thereby the coated article body is played a protective role.Coating generally includes epoxypaint, amino-resin coating, phenolic resin paint, phthalic resin coating etc.Wherein epoxy coating has the excellent chemical resistance, and alkaline resistance properties is particularly outstanding, is excellent protective system, and metal, glass, pottery etc. are all had good sticking power, is widely used in the application of iron and steel framework, building, vehicle, furniture etc.
Epoxypaint generally includes resin Composition and curing agent component; Wherein because aliphatic polyamine class solidifying agent solidification value is lower; So the solidifying agent that existing epoxypaint uses is aliphatic polyamine class solidifying agent; With being coated on the coated object surface behind resin Composition and the curing agent component proportional mixing, dry and hard film forming is attached to body surface behind resin and the solidifying agent generation curing reaction before using.Application number is that 200410050479.6 Chinese patent document discloses a kind of ocean heavy-duty coating; It is made up of A, two kinds of components of B; Wherein the A component is phenolic aldehyde amine curing agent and ketoimine, and B comprises auxiliary agents such as epoxy resin and properties-correcting agent, sequestrant, dispersion agent, filler.Though this coating has preservative effect preferably, but the curing reaction that A, B component mixing back resin and solidifying agent are taken place is incomplete, so still contains the part unhindered amina after the coating film forming, and toxicity is bigger, is not suitable for the application of drinking water pipeline.
Summary of the invention
The technical problem that the present invention solves is, a kind of nontoxic epoxypaint is provided, and comprises resin Composition and curing agent component, and said resin Composition comprises:
Epoxy equivalent (weight) is epoxy resin 25wt%～40wt% of 235～265
Epoxy equivalent (weight) is epoxy resin 3wt%～6.5wt% of 170～195
Dispersion agent 0.2wt%～0.7wt%
Flow agent 1wt%～2wt%
Thinner 5wt%～12wt%
Filler 50wt%～65wt%
Said curing agent component comprises:
Phenolic aldehyde amine modified firming agent 18wt%～26wt%
Cashew nut oil modified pnenolic aldehyde amine hardener 52wt%～66wt%
YLENE 10wt%～25wt%
The weight ratio of said epoxy resin ingredient and said curing agent component is 6～7: 1.
Preferably, said epoxy resin is bisphenol A epoxide resin.
Preferably, said dispersion agent is the mixing solutions of unsaturated polyamine and acid polyester salt.
Preferably, said flow agent is inorganic modified Viscotrol C.
Preferably, said filler is one or more in white titanium pigment, mica powder, talcum powder or the silica powder.
Preferably, said thinner is the mixing solutions of YLENE and propyl carbinol.
Preferably, YLENE and propyl carbinol blending ratio are 3～6: 7～9 by weight.
The present invention also provides a kind of preparation method of epoxypaint, comprising:
Preparation resin Composition: 5～12 parts of thinners are provided; Get the thinner of 30wt% and be that 235～265 epoxy resin and 3～6.5 parts of epoxy equivalent (weight)s are to disperse after 170～195 epoxy resin mixes with 25～40 parts of epoxy equivalent (weight)s; Add 0.2～0.7 part of dispersion agent, 1～2 part of flow agent and 50～64 parts of fillers then and disperse once more, the dispersion back adds remaining 70wt% thinner and stirs;
Preparation curing agent component: the phenolic aldehyde amine modified firming agent of 10 parts～25 parts YLENE and 52～66 parts of cashew nut oil modified phenolic aldehyde amine and 18～26 parts is mixed and the dispersion afterwards that stirs;
With resin Composition and curing agent component according to 6～7: 1 weight ratio is mixed and is obtained epoxypaint.
Preferably, said epoxy resin is bisphenol A epoxide resin.
Preferably, said thinner is the mixing solutions of YLENE and propyl carbinol.
The invention provides a kind of epoxypaint, the epoxy resin in the resin Composition of said coating is that epoxy equivalent (weight) is the composite of 235～265 and 170～195 epoxy resin, and molecular weight is less, and cross-linking density is big; Contain phenolic aldehyde amine modified firming agent and cashew nut oil modified pnenolic aldehyde amine hardener in the solidifying agent, wherein cashew nut oil modified pnenolic aldehyde amine hardener does not contain phenol, is natural component synthetic modified amine; The modified solidified adding of phenolic aldehyde amine can reduce solidification value, and still has preferably effect admittedly at the environment of humidity.Coating uses preceding with behind resin Composition and the curing agent component proportional mixing; The curing reaction that the resin of said ratio and solidifying agent take place is fast and complete; Do not have unhindered amina in the coating system, satisfy water establishing of Drinking Water transmission & distribution and protective material safety evaluation standard through the said coating of test; The paint film that forms is fine and close, and the water vapor permeable rate is low, has excellent antiseptic property; Simultaneously, because the carbochain of the solidifying agent that uses is longer, thereby make the paint film that obtains have excellent flexibility; Solidifying agent contains phenyl ring, thereby makes the hardness of paint film that obtains high, and the paint film mechanical property is good, long service life.
Embodiment
In order further to understand the present invention, below in conjunction with embodiment the preferred embodiment of the invention is described, describe just to further specifying feature and advantage of the present invention but should be appreciated that these, rather than to the restriction of claim of the present invention.
The embodiment of the invention discloses a kind of epoxy resin and be coated with, comprise resin Composition and curing agent component, the composition of resin Composition and each component concentration are following:
Epoxy equivalent (weight) is epoxy resin 25wt%～40wt% of 235～265
Epoxy equivalent (weight) is epoxy resin 3wt%～6.5wt% of 170～195
Dispersion agent 0.2wt%～0.7wt%
Flow agent 1wt%～2wt%
Thinner 5wt%～12wt%
Filler 50wt%～6wt%
Curing agent component and each component concentration are following:
Phenolic aldehyde amine modified firming agent 18wt%～26wt%
Cashew nut oil modified pnenolic aldehyde amine hardener 52wt%～66wt%
YLENE 10wt%～25wt%
The weight ratio of said epoxy resin ingredient and said curing agent component is 6～7: 1.
It is two kinds of epoxy resin of 235～265 and 170～195 that resin Composition in the epoxy coating provided by the invention contains epoxy equivalent (weight); Two kinds of molecular weight of epoxy resin are less; Cross-linking density is big behind the curing reaction, and above-mentioned epoxy resin includes but not limited to: bisphenol A epoxide resin, aliphatic epoxy resin, glycidyl epoxies, glycidyl amine epoxy resin or dimer acid modified epoxy resin, and the present invention preferably adopts bisphenol A epoxide resin; It contains than poly-hydroxy; Have stronger polarity and chemical activity, be prone to and the effect of coated article body, sticking power is stronger.Epoxy equivalent (weight) is that the content of 235～265 epoxy resin is 25wt%～40wt% in the resin Composition; Epoxy equivalent (weight) is that the content of 170～195 epoxy tree is 3wt%～6.5wt%; Two kinds of resin contents are low excessively, then are prone to cause curing reaction incomplete, contain unhindered amina in the coating system; Two kinds of resins are as if too high levels, and then coating system viscosity is bigger, influences curing reaction speed and solidification value.
Dispersion agent preferably adopts the mixing solutions of unsaturated polyamine and acid polyester salt; Flow agent preferably adopts inorganic modified Viscotrol C; Filler preferably adopts one or more in white titanium pigment, mica powder, talcum powder and the silica powder, plays the enhanced effect; Thinner preferably adopts the mixing solutions of YLENE and propyl carbinol, and blending ratio is preferably 7～9: 3～6 by weight, and the reactive group in the thinner can promote the epoxy resin open loop, plays promoter action to setting up perfect cross-linked network.
The solidifying agent that the present invention adopts contains cashew nut oil modified phenolic aldehyde amine and phenolic aldehyde amine modified firming agent, and cashew nut oil modified phenolic aldehyde amine does not contain phenol, is natural components synthetic modified amine; It is the raw material that obtains U.S. FDA and NSF authentication; Be the amine curing agent that can be used for producing the corrosion-resistant epoxy paint that contacts with food or tap water, its viscosity is low, and rate of drying is fast; Low-temperature curable, and excellent water-fast, rustless property are arranged.The phenolic aldehyde amine modified firming agent is one type of ideal epoxy resin ambient cure agent; Because its molecular weight is lower; Thereby viscosity is lower, and the compatibility of itself and epoxy resin is good, and wellability is strong; Curing speed is fast, and can be at-18 ℃, humidity greater than 80% with wait the epoxy resin that solidifies various models in the multiple environment under water.The carbochain of above-mentioned solidifying agent is longer, and the paint film that therefore obtains has excellent flexibility; Above-mentioned solidifying agent contains phenyl ring, and the hardness of paint film that therefore obtains is high, and the paint film mechanical property is good, long service life.The content of cashew nut oil modified phenolic amine hardener is 52wt%～66wt% in the curing agent component, and the content of cashew nut oil modified pnenolic aldehyde amine hardener is 52wt%～66wt%, and if above-mentioned two kinds of curing agent content then are prone to residual unhindered amina too high in curing reaction; If above-mentioned two kinds of curing agent content make that then the solidification value of coating is higher low excessively.
YLENE all has solvability preferably to above-mentioned epoxy resin and solidifying agent.When with resin Composition with after curing agent component mixes; Epoxy resin and solidifying agent generation curing reaction; The epoxy resin of said ratio and solidifying agent system curing reaction when being cured reaction is fast and complete; Have no unhindered amina, thereby make product itself nontoxic, can be used for food such as tap water, food factory, dairies, milk transport pipe, the brew-house directly pipeline and the equipment of contact; The paint film that forms has perfect tridimensional network, and paint film is fine and close, and the water vapor permeable rate is low, has excellent antiseptic property, can be immersed in clear water and the salt solution, and anti-cathodic protection.Can be used for heavy anticorrosion occasion such as boats and ships and use the hydraulic pressure storehouse, water and sewage work etc.
The present invention also provides a kind of method of epoxypaint, comprising:
A, 5～12 parts of thinners are provided; Get the thinner of 30wt% and be that 235～265 epoxy resin and 3～6.5 parts of epoxy equivalent (weight)s are to disperse after 170～195 epoxy resin mixes with 25～40 parts of epoxy equivalent (weight)s; Add 0.2～0.7 part of dispersion agent, 1～2 part of flow agent and 50～64 parts of fillers then and disperse once more, the dispersion back adds remaining 70wt% thinner and stirs;
B, the phenolic aldehyde amine modified firming agent of 10 parts～25 parts YLENE and 52～66 parts of cashew nut oil modified phenolic aldehyde amine and 18～26 parts is mixed and the back that stirs disperses;
C, with resin Composition and curing agent component according to 6～7: 1 weight ratio is mixed and is obtained epoxypaint.
Step a is the preparation resin Composition; Thinner in the resin Composition preferably adopts the mixing solutions of YLENE and propyl carbinol; Blending ratio is preferably 3～6: 7～9 by weight, and the reactive group in the thinner can promote the epoxy resin open loop, plays promoter action to setting up perfect cross-linked network.The epoxy resin of selecting for use includes but not limited to: bisphenol A epoxide resin, aliphatic epoxy resin, glycidyl epoxies, glycidyl amine epoxy resin or dimer acid modified epoxy resin; The present invention preferably adopts bisphenol A epoxide resin; It contains than poly-hydroxy; Have stronger polarity and chemical activity, be easy to the effect of coated article body, sticking power is stronger.Powder preferably adopts the mixing solutions of unsaturated polyamine and acid polyester salt, and flow agent preferably adopts inorganic modified Viscotrol C, and filler preferably adopts one or more in white titanium pigment, mica powder, talcum powder and the silica powder, plays the enhanced effect.Among the step a thinner and mixed with resin are carried out dispersive speed and be preferably 300rpm～600rpm, add dispersion agent, flow agent and filler again and carry out dispersive speed and be preferably 100rpm～1300rpm.Disperse to use method well known to those skilled in the art to disperse above-mentioned raw materials, the present invention does not have special restriction to this.
Step b is the preparation curing agent component, and the rate of dispersion in this step is preferably 600rpm～900rpm.
Before the use, the resin Composition and the curing agent component proportional mixing of step a and b configuration can be carried out application, can use method well known to those skilled in the art to mix, the present invention does not have special restriction to this.
In order further to understand the present invention, epoxypaint provided by the invention and preparation method thereof is described below in conjunction with embodiment.Epoxy resin resin a in following examples provides by Anglo-Dutch Royal Shell Group, and oxirane value is 0.38～0.425; Epoxy resin b is provided by Huntsman company, and oxirane value is 0.52～0.55; Dispersion agent is provided by BYK company; Inorganic modified Viscotrol C is provided by ELEMENTIS company; The phenolic aldehyde amine modified firming agent is provided by Cardolite company; Cashew nut oil modified pnenolic aldehyde amine hardener is provided by Cardolite company.
Embodiment 1
The YLENE of 3.6kg mixed with the propyl carbinol of 6.6kg obtain thinner; In dispersion machine, add epoxy resin a, 9.5kg epoxy resin b and the 3kg thinner of 25.5kg and carry out the low speed dispersion; It is 500rpm that dispersing speed is set; Low speed disperses to start water coolant after 5 minutes, and the talcum powder that adds the inorganic modified Viscotrol C of dispersion agent, 1.5kg, 15kg white titanium pigment, 7.5kg mica powder, 13.2kg silica powder and the 17kg of 0.6kg again carries out high speed dispersion, and it is 1100rpm that dispersing speed is set; High speed dispersion adds the 7.2kg thinner and stirs after 45 minutes, obtain resin Composition;
15.5kg YLENE is mixed with cashew nut oil modified phenolic aldehyde amine of 59kg and 25.5kg phenolic aldehyde amine modified firming agent and the back that stirs disperses in the dispersion machine middling speed, and it is 700rpm that rotating speed is set, and middling speed obtained curing agent component after 20 minutes;
Before coating uses with resin Composition and curing agent component according to 6～7: 1 weight ratio is mixed just can carry out application.
Embodiment 2
The coating layoutprocedure is identical with embodiment 1, and epoxypaint component and each component concentration that present embodiment provides are following:
Resin Composition is following:
Epoxy resin a 31.10kg
Epoxy resin b 4.50kg
Dispersion agent 0.40kg
Inorganic modified Viscotrol C 1.9kg
White titanium pigment 16.00kg
Mica powder 7.50kg
Talcum powder 16.00kg
Silica powder 15.20kg
YLENE 2.60kg
Propyl carbinol 4.80kg
Curing agent component is following:
Phenolic aldehyde amine modified firming agent 19.50kg
Cashew nut oil modified pnenolic aldehyde amine hardener 65.00kg
YLENE 15.50kg
Embodiment 3
The coating layoutprocedure is identical with embodiment 1, and epoxypaint component and each component concentration that present embodiment provides are following:
Resin Composition is following:
Epoxy resin a 37.6kg
Epoxy resin b 4.50kg
Dispersion agent 0.50kg
Inorganic modified Viscotrol C 1.2kg
White titanium pigment 26.00kg
Silica powder 25.00kg
YLENE 2.20kg
Propyl carbinol 3.00kg
Curing agent component is following:
Phenolic aldehyde amine modified firming agent 23.00kg
Cashew nut oil modified pnenolic aldehyde amine hardener 62.00kg
YLENE 15.00kg
The epoxy coating of embodiment 1 to 3 preparation is carried out Drinking Water transmission & distribution wetting system and protective material security test, and testing standard is GB/T 17219, and test result is listed in table 1.
The epoxy coating of embodiment 1 to 3 preparation is carried out mechanical property and corrosion resistance nature test, and test result is listed in table 2.
Table 1 Drinking Water transmission & distribution wetting system and protective material security test
| Test event | Embodiment 1 | Embodiment 2 | Embodiment 3 |
| Colourity | 2 | 3 | 3 |
| Opacity | 0.33 | 0.35 | 0.33 |
| Smelly and the flavor | Do not have | Do not have | Do not have |
| The naked eyes visible | Do not have | Do not have | Do not have |
| PH，mg/L | 8.05 | 8.05 | 8.05 |
| Iron, mg/L | 0.003 | 0.0035 | 0.0035 |
| Manganese, mg/L | 0.0015 | 0.002 | 0.0015 |
| Copper, mg/L | 0.0004 | 0.0004 | 0.0004 |
| Zinc, mg/L | 0.0015 | 0.001 | 0.001 |
| Volatilization amine (in phenol), mg/L | 0 | 0 | 0 |
| Arsenic, mg/L | 0.0004 | 0.0004 | 0.0004 |
| Mercury, mg/L | 0.00005 | 0.00008 | 0.00005 |
| Cadmium, mg/L | 0.0002 | 0.0002 | 0.0002 |
| Lead, mg/L | 0 | 0 | 0 |
| Silver, mg/L | 0.0001 | 0.0001 | 0.00015 |
| Fluorochemical, mg/L | 0.03 | 0.04 | 0.04 |
| Nitrate nitrogen (in nitrogen), mg/L | 0.3 | 0.3 | 0.3 |
| Chromium (sexavalence), mg/L | 0.003 | 0.003 | 0.003 |
| Potassium permanganate consumption is (with O 2Meter), mg/L | 0.38 | 0.40 | 0.39 |
| Chloroform, μ g/L | 3.06 | 3.05 | 3.06 |
| Tetracol phenixin, μ g/L | 0.05 | 0.05 | 0.05 |
| Benzo (a) pyrene, μ g/L | 0.006 | 0.008 | 0.008 |
Table 2 mechanical property and corrosion resistance nature test
Can know by The above results; Epoxy coating provided by the invention satisfies GB/T 17219-1998 Drinking Water transmission & distribution wetting system and protective material safety evaluation standard, can be used for food such as tap water, food factory, dairies, milk transport pipe, the brew-house directly pipeline and the equipment of contact.Paint film has excellent mechanical property and corrosion resistance nature, can be used for heavy anticorrosion occasion such as boats and ships and uses hydraulic pressure storehouse, fields such as water and sewage work.
The explanation of above embodiment just is used for helping to understand method of the present invention and core concept thereof.Should be pointed out that for those skilled in the art, under the prerequisite that does not break away from the principle of the invention, can also carry out some improvement and modification to the present invention, these improvement and modification also fall in the protection domain of claim of the present invention.
To the above-mentioned explanation of the disclosed embodiments, make this area professional and technical personnel can realize or use the present invention.Multiple modification to these embodiment will be conspicuous concerning those skilled in the art, and defined General Principle can realize under the situation that does not break away from the spirit or scope of the present invention in other embodiments among this paper.Therefore, the present invention will can not be restricted to these embodiment shown in this paper, but will meet and principle disclosed herein and features of novelty the wideest corresponding to scope.
Claims (8)
1. an epoxypaint comprises resin Composition and curing agent component, and said resin Composition comprises:
The weight ratio of said resin Composition and said curing agent component is 6 ~ 7: 1.
2. epoxypaint according to claim 1 is characterized in that, said dispersion agent is the mixing solutions of unsaturated polyamine and acid polyester salt.
3. epoxypaint according to claim 1 is characterized in that, said flow agent is inorganic modified Viscotrol C.
4. epoxypaint according to claim 1 is characterized in that, said filler is one or more in white titanium pigment, mica powder, talcum powder or the silica powder.
5. epoxypaint according to claim 1 is characterized in that, said thinner is the mixing solutions of YLENE and propyl carbinol.
6. epoxypaint according to claim 5 is characterized in that, YLENE and propyl carbinol blending ratio are 3 ~ 6: 7 ~ 9 by weight.
7. the preparation method of an epoxypaint comprises:
Preparation resin Composition: 5 ~ 12 parts of thinners are provided; Get the thinner of 30wt% and be that 235 ~ 265 bisphenol A epoxide resin and 3 ~ 6.5 parts of epoxy equivalent (weight)s are to disperse after 170 ~ 195 bisphenol A epoxide resin mixes with 25 ~ 40 parts of epoxy equivalent (weight)s, dispersive speed is 300rpm ~ 600rpm; Add 0.2 ~ 0.7 part of dispersion agent, 1 ~ 2 part of flow agent and 50 ~ 64 parts of fillers then and disperse once more, dispersive speed is 100rpm ~ 1300rpm; The dispersion back adds remaining 70wt% thinner and stirs;
The preparation curing agent component: the phenolic aldehyde amine modified firming agent of 10 parts ~ 25 parts YLENE and 52 ~ 66 parts of cashew nut oil modified phenolic aldehyde amine and 18 ~ 26 parts is mixed and the dispersion afterwards that stirs, and dispersive speed is 600rpm ~ 900rpm;
With resin Composition and curing agent component according to 6 ~ 7: 1 weight ratio is mixed and is obtained epoxypaint.
8. method according to claim 7 is characterized in that, said thinner is the mixing solutions of YLENE and propyl carbinol.
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| CN103265865B (en) * | 2013-04-24 | 2015-05-06 | 瑞安市德仕节能材料科技有限公司 | Production technology of water-soluble volcanic ash paint |
| KR20160007493A (en) * | 2013-05-10 | 2016-01-20 | 블루 큐브 아이피 엘엘씨 | Epoxy resin compositions |
| JP6051194B2 (en) | 2013-12-11 | 2016-12-27 | ダウ グローバル テクノロジーズ エルエルシー | Coating system, method of applying the coating system, and article comprising the coating system |
| CN106010142B (en) * | 2016-08-08 | 2017-12-19 | 中山市长博电子绝缘材料有限公司 | A kind of wear-resisting single component epoxy coating of dual cure and preparation method thereof and application method |
| CN107057037A (en) * | 2017-04-21 | 2017-08-18 | 深圳市景方盈科技有限公司 | Epoxy resin manufacture method |
| CN107629195B (en) * | 2017-11-03 | 2020-01-10 | 昆明迈泽科技有限公司 | Preparation method and application of phosphate modified cashew nut oil curing agent |
| CN113429545A (en) * | 2021-07-06 | 2021-09-24 | 湖北铁神新材料有限公司 | Water-based epoxy phosphate resin and edible oil storage tank inner wall coating and preparation method thereof |
| CN116120871B (en) * | 2023-01-10 | 2024-09-13 | 安徽牛元新材料有限公司 | Smell-removing elastic dry-hanging adhesive and preparation method thereof |
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