CN103254736B - A kind of have Polyaniline powder paint of acid resistance self-repair function and preparation method thereof - Google Patents
A kind of have Polyaniline powder paint of acid resistance self-repair function and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to a kind of Polyaniline powder paint with acid resistance self-repair function, its raw material forms component and parts by weight are respectively: special epoxy resin 450 ~ 550 parts; 80 ~ 140 parts, solidifying agent; Polyaniline 5 ~ 100 parts; Color stuffing 200 ~ 250 parts; Auxiliary agent 30 ~ 50 parts.Powder coating of the present invention contains the coating of a certain amount of polyaniline, in acid condition, there is anodic oxidation reactions, quick recovery surface passivation layer, even if corrosive deposit immerses, passivation layer can as the second barrier, also the generation of corrosion can be hindered, ensure that antiseptic property and the self-healing properties of coating, warping resistance, snappiness significantly improve, and have the characteristic of improved corrosion, scratch resistance capability; The selfreparing passive behavior of the barrier property of common coating and polyaniline combines by this powder coating, realize once getting final product thick painting, construction is simple, avoid the workpiece after coating in construction process after breakage, from the hidden danger of breaking point starting point corrosion, sticking power, the corrosion resistance of coating also have passed GB correlation detection.<!--1-->
Description
Technical field
The invention belongs to paint field, relate to decorative powder coatings, especially a kind of have Polyaniline powder paint of acid resistance self-repair function and preparation method thereof.
Background technology
1985, DeBerry finds, in acidic medium, can make stainless steel surface active passivation and anticorrosion with the polyaniline film of electrochemical process synthesis, this feature attracts attention, and from then on people start the applied research of conducting polymer film in corrosion prevention field.
1991, Los Alamos National Laboratories (IANL) and the NASA (NASA) of the U.S. report conductive polyaniline to soft steel preservative activity, the Kennedy Space launching centre of NASA is located in the coastal region of seriously corroded, there was dampness in the air in there, salt air corrosion is serious, and each rocket launching all will produce the high temperature HC1 gas of nearly 13 tons, have a strong impact on launcher and other facility work-ing life.They find, polyaniline is coated in the inwall of rocket launching tower, high temperature acid mist can be avoided the corrosion of launching tower, effect is very good.Kennedy Space launching centre and GeoTech company contract, and authorize GeoTech manufacturer product to be called the polyaniline anti-corrosive paint of Catiz.The commercial value of anticorrosive polyaniline performance is seen some from this.
The antiseptic property of polyaniline is not only a simple passivation layer, redox reaction occurs at the interface of polyaniline and iron, generates the compound of a kind of Fe-PANI; The oxidizing potential of this compound, higher than the oxidizing potential of independent PANI, promotes the reduction of oxygen, thus compensate for the electric charge consumed because of the dissolving of iron, the current potential of iron is stabilized in passivation region, can reduces the dissolution rate of metal with katalysis.
Polyaniline is due to the strong rigidity of its chain and the strong interaction of interchain, and make its solvability extreme difference, be dissolved in any solvent hardly, the cohesiveness of pure polyaniline to metal is very poor.These shortcomings significantly limit polyaniline application technically.
Common protective system is only corrosive medium and metal base are isolated, and blocks the contact of corrosive deposit and metal, thus reaches anticorrosion object.But its preservative effect must be subject to the quality of pre-treatment and the impact of coating density, common coating presents loose and porous structure under an electron microscope mostly, and corrosive medium often immerses from comparatively macrovoid, thus corroding metal base material.
By retrieval, not yet find the patent publication us relevant to patent application of the present invention.
At present, domestic not yet discovery meets the powder coating product of above-mentioned functions.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art part, a kind of improved corrosion, scratch resistance capability are provided, strong adhesion there is Polyaniline powder paint of acid resistance self-repair function and preparation method thereof, this preparation method's method is simple, easy to operate, save production cost, improve the economic benefit of enterprise.
The technical solution adopted for the present invention to solve the technical problems is:
Have a Polyaniline powder paint for acid resistance self-repair function, its raw material forms component and parts by weight are respectively:
And, the mixture that described special epoxy resin forms for modified bisphenol A type epoxy resin, bisphenol A-type high molecular solid epoxy and o-cresol formaldehyde epoxy resin, modified bisphenol A type epoxy resin: bisphenol A-type high molecular solid epoxy: the mass ratio of o-cresol formaldehyde epoxy resin is: 280 ~ 320:130 ~ 180:30 ~ 50.
And, described modified bisphenol A type epoxy resin: bisphenol A-type high molecular solid epoxy: the mass ratio of o-cresol formaldehyde epoxy resin is 300:150:35.
And described auxiliary agent is the mixture of flow agent, brightening agent, defoamer, and its parts by weight are as follows:
Flow agent: 16 ~ 22 parts;
Anti-interference agent: 10 ~ 20 parts;
Pore eliminator: 4 ~ 8 parts.
And the mass ratio of the mixture of described flow agent, brightening agent, defoamer is 9:7:3.
And described polyaniline molecule structural formula is:
And described solidifying agent is imidazoles or phenols curing agent.
And, the linear resin that described solidifying agent is is end group with glyoxal ethyline, dihydroxyphenyl propane.
And described color stuffing is the mixture of one or more in common Rutile type Titanium Dioxide, carbon black, silicon powder or process white.
There is the preparation method of the Polyaniline powder paint of acid resistance self-repair function as above, it is characterized in that: step is as follows:
(1) preparation of polyaniline:
1. emulsion polymerization synthesized polyaniline technique: add in the reactor in aniline: the ratio of the amount of substance of dodecylbenzene is that the ratio of 2:1 is for adding aniline and dodecylbenzene, water, dimethylbenzene is added successively after mixing, abundant stirring, to obtaining transparent emulsion;
2. then in transparent emulsion in ammonium persulphate: the ratio of the amount of substance of aniline is that the ratio of 1:1 drips ammonium persulphate (NH
4)
2s
2o
8the aqueous solution, system color slowly deepens, and keeps system temperature 0 ~ 20 DEG C, continues stirring 30 minutes, after during static storing 24, then adds acetone breakdown of emulsion, with ethanol or acetone repetitive scrubbing 3 ~ 4 times, removes ethanol or acetone, filters and to obtain precipitation;
3. use water, dodecylbenzenesulfonic acid solution washing precipitation substantially colourless to filtrate successively, vacuum-drying 48h at 40 DEG C, obtain the polyaniline powder adulterated;
(2) preparation of powder coating:
The polyaniline powder of synthesis in step (1) and specific epoxy, solidifying agent, auxiliary agent, color stuffing are pressed formula rate to be weighed accurately, stir, extrude extrusion temperature 80 ~ 90 DEG C through twin screw extruder again, compressing tablet, Crushing of Ultrafine, to sieve, the Polyaniline powder paint of acid resistance self-repair function must be had.
Advantage of the present invention and positively effect are:
1, powder coating of the present invention contains the coating of a certain amount of polyaniline, in acid condition, there is anodic oxidation reactions, quick recovery surface passivation layer, even if corrosive deposit immerses, passivation layer can as the second barrier, also the generation of corrosion can be hindered, ensure that antiseptic property and the self-healing properties of coating, warping resistance, snappiness significantly improve, and have the characteristic of improved corrosion, scratch resistance capability; The selfreparing passive behavior of the barrier property of common coating and polyaniline combines by this powder coating, realize once getting final product thick painting, construction is simple, avoid the workpiece after coating in construction process after breakage, from the hidden danger of breaking point starting point corrosion, sticking power, the corrosion resistance of coating also have passed GB correlation detection.
2, powder coating of the present invention adopts the oblong link epoxy resins of repeating unit 4 ~ 7, the mean polymerisation degree of contained epoxy resin controls between 4 ~ 9, the epoxy-resin systems that different kinds of molecules structure is different, to arrange in pairs or groups by a certain percentage use, macromole complementary networks structure, form fine and close coating, be equipped with heavy antisepsis type o-cresol-formaldehyde resin, instead of the liquid epoxy that paint adopts and add polyamine curing system, not only containing more phenyl ring and hydroxyl in novolac epoxy molecular structure, and have longer flexible chain, aim at double antiseptic powder coating design, there is fabulous intermiscibility, reactive behavior is high, there is very strong adhesive power, can fast setting, cross-linking density is high, film has remarkable rigidity and humidity resistance, chemical-resistant, solvent resistance, resistance to cathodic disbonding, levelling property and snappiness, the mechanical propertys such as shock resistance.
3, powder coating of the present invention adopts phenolic hydroxyl group long-chain solidifying agent, with modified imidazole catalytic curing in the hope of reaching quick-setting target; Coatings additive(s) is 788 flow agents, 701B brightening agent, benzoic mixture, is more conducive to form fine and close smooth surface, reduces coating porosity; Linear resin (the appearance white crystal that solidifying agent adopts glyoxal ethyline, dihydroxyphenyl propane is end group, fusing point DEG C 143.0 ~ 146.0, content % >=99.5), object is for making coating low-temperature fast-curing and have heavy antisepsis function, to improve film flexibility, increase the probability being wound around, embedding, the polyhydroxy structure that solidifying agent has simultaneously also improves the sticking power to base material.
4, powder coating color stuffing of the present invention is only for color matching is used, critical impact is not produced on antiseptic property, different coating color adopts different pigment collocation, pigment variety also changes thereupon, color stuffing adopts one or more in common Rutile type Titanium Dioxide, carbon black, torispherical silicon powder or process white, cheap and easy to get, also have concurrently and improve coatingsurface hardness, improve the effect of resistance to marring.
In the preparation method of 5, powder coating of the present invention, the polymerization yield rate of the polyaniline that the explained hereafter of synthesized polyaniline obtains is greater than 80%, the specific conductivity of polyaniline is greater than 1S/cm, and, the plurality of advantages such as emulsion polymerization rate of polymerization is high, molecular weight of product is high, have good thermostability and particle size is even, method is simple, easy to operate, save production cost, improve the economic benefit of enterprise.
Accompanying drawing explanation
Fig. 1 is that floating coat of the present invention damages and self-regeneration figure (Original: the original state of testing plate; SI: testing plate is through 12% salt solution, and 75 DEG C are soaked the states after 290 hours; Ov: testing plate is through the state of 80 DEG C of bakings after 72 hours); (low frequency, the preservative effect of the higher coating of resistance when namely X-coordinate is-1 is better).
Wherein, Fig. 1-1 is common coating and contains polyaniline coating initial state; Wherein, Fig. 1-2 is that after 3 days, common coating starts to corrode appearance a little; Fig. 1-3 is that after 12 days, common coating is by thorough corrosion failure, and Fig. 1-4 is 15 days post-dryings, and good containing polyaniline coating self-regeneration, common coating cannot be repaired.
Embodiment
Below by specific embodiment, the invention will be further described, and following examples are descriptive, is not determinate, can not limit protection scope of the present invention with this.
The method used in the present invention if no special instructions, is ordinary method; The reagent used in the present invention if no special instructions, is conventional reagent.
The principle that powder coating of the present invention has self-regeneration function is:
Electrically conductive polyaniline has excellent environmental stability, higher electroconductibility, polyaniline paint can form oxide compound in metallic surface, when coatingsurface has cut or cavity, polyaniline can repair the chemical aging between metal or oxide compound, the coating at exposed position still has good preservative effect, the advantage that this characteristic has other coating incomparable; Under acid (acid rain) environment, the corrosion resistance coating having the coating of polyaniline to compare not this component exceeds 100 times.Electrically conductive polyaniline has become one of conducting polymer having application prospect most that industry is generally acknowledged.
Powder coating of the present invention has certain conductive characteristic, when the coating of metallic surface has defect, polyaniline can play a kind of catalytic deactivation effect to this position, in acid condition, polyaniline brings out iron passivation, and the interface of iron and polyaniline can produce an electric field, and the direction of this electric field is contrary with electron transmission direction, hinder electronics from metal to the transmission of oxidizing substance, be equivalent to the barrier action of an electron transmission; Polyaniline and metal form compound, and current potential is raised, thus have promoted the reduction of oxygen, make because the dissolving of metal and the electric charge of loss is compensated, metal current potential is stabilized in passivation region, decreases the dissolution rate of metal, quick recovery surface passivation layer, thus play preservative activity.Conventional coating can not form this electric field as epoxy resin or urethane, does not thus have self-repair function.
The present invention, by adulterating (being adulterated by Witco 1298 Soft Acid) in emulsion polymerization process, is adopted twin-screw extrusion internally mix technology, while improving the conductivity of polyaniline, too increases its intermiscibility in application process.Adopting joins in epoxide powder coating by polyaniline, by electrostatic spraying, at-60kV, toasts 20min at 140 DEG C, and under hot salt condition, test electrochemical impedance spectroscopy, have studied its Corrosion Protection, and made SaltSprayTest.The blended coating of polyaniline processes 1400h under 65 DEG C of hot salt conditions, does not change.When artificial damage, this coatings goes out good self-reparing capability, and even under the hot salt condition continued, base material does not also get rusty.This is because the crosslinked of polyaniline improves isolating and protecting and self-repairability, prevents the corrosion of base material, DSC(dsc) research confirm this explanation.
The special epoxy resin used in the present invention adopts the oblong link epoxy resins of repeating unit 4 ~ 7, for the epoxy-resin systems that different kinds of molecules structure is different, to arrange in pairs or groups by a certain percentage use, macromole complementary networks structure, form fine and close coating, the mean polymerisation degree of contained epoxy resin should control between 4 ~ 9, can be such as (as the CYD804L of Ba Ling petrochemical industry by modified bisphenol A type epoxy resin, glycol modified bisphenol type epoxy), bisphenol A-type high molecular solid epoxy (as NPES-907) and o-cresol formaldehyde epoxy resin the mixture that forms, its parts by weight are as follows:
Modified bisphenol A type epoxy resin 280 ~ 320 parts;
Bisphenol A-type high molecular solid epoxy 130 ~ 180 parts;
O-cresol formaldehyde epoxy resin 30 ~ 50 parts.
The solidifying agent used can be 2--phenylimidazole and novolac class solidifying agent (appearance white crystal, softening temperature is in order to 85 ~ 95, content % >=99.5)), such as 2-phenylimidazole, dihydroxyphenyl propane are the linear resin of end group, A-601, the V-205 of such as Shaanxi gold occasion chemical industry, the Amanda-969A etc. of grand celebration celebrating Shandong chemical industry.
Embodiment 1
Have a Polyaniline powder paint for acid resistance self-repair function, its raw material forms component and parts by weight are respectively:
The above-mentioned step with the preparation method of the Polyaniline powder paint of acid resistance self-repair function is as follows:
(1) preparation of polyaniline:
1. emulsion polymerization synthesized polyaniline technique: add aniline and dodecylbenzene (ratio of the amount of substance of the two is 2:1) in the reactor, add water after mixing successively, (two is all solvent to dimethylbenzene, do not participate in reaction, appropriate), abundant stirring, to obtaining transparent emulsion;
2. then in transparent emulsion, ammonium persulphate (NH is dripped
4)
2s
2o
8the aqueous solution (ammonium persulphate is 1:1 with the ratio of the amount of aniline), system color slowly deepens, keep system temperature 0 ~ 20 DEG C, continue stirring 30 minutes, after during static storing 24, then add proper amount of acetone breakdown of emulsion, with appropriate ethanol or acetone repetitive scrubbing 3 ~ 4 times, remove ethanol or acetone, filter to obtain precipitation;
3. use water, dodecylbenzenesulfonic acid solution washing precipitation substantially colourless to filtrate successively, vacuum-drying 48h at 40 DEG C, obtain the polyaniline powder adulterated; The molecular structural formula of preparation-obtained polyaniline is:
(2) preparation of powder coating:
The polyaniline powder of synthesis in step (1) and specific epoxy, solidifying agent, auxiliary agent, color stuffing are pressed formula rate to be weighed accurately, pour high speed mixer into, forcing machine is added to after dry blending stirs, conventional melting, mixing, cooling, compressing tablet is carried out extrusion temperature 80 ~ 90 DEG C again through twin screw extruder, again through pulverizer pulverizing, classification, sieve, pack, namely become powder coating final product.
Embodiment 2
Have a Polyaniline powder paint for acid resistance self-repair function, its raw material forms component and parts by weight are respectively:
The above-mentioned preparation method with the Polyaniline powder paint of acid resistance self-repair function is with embodiment 1.
Embodiment 3
Have a Polyaniline powder paint for acid resistance self-repair function, its raw material forms component and parts by weight are respectively:
The above-mentioned preparation method with the Polyaniline powder paint of acid resistance self-repair function is with embodiment 1.
Embodiment 4
Have a Polyaniline powder paint for acid resistance self-repair function, its raw material forms component and parts by weight are respectively:
The above-mentioned preparation method with the Polyaniline powder paint of acid resistance self-repair function is with embodiment 1.
The practical application effect of powder coating of the present invention and test situation:
In acidic medium, there is the carbon steel of polyaniline rete than there is no the solidity to corrosion of rete and exceed 100 times; And be in the medium of 7 in pH value, there is the carbon steel of polyaniline rete only to exceed 2 times than the solidity to corrosion of reduction-state; In the seawater of pH value 8.0 ~ 9.4, not evidence suggests that polyaniline has good antiseptic property.This structure that can be interpreted as polyaniline is relevant with pH value.So experiment conclusion shows, polyaniline coating only just can put out the antiseptic property of its excellence to good use in sour environment, and in alkaline environment, mainly also by epoxy coat.
By different application modes and analysis test method (such as, in ASTM to the examination criteria method of coating; Electrochemical test method measures open circuit potential, corrosion potential, corrosion current and polarization impedance etc.; The structure of the methods analyst matallic surface layers such as XPS and SEM and chemical composition) have studied polyaniline paint to the anticorrosion ability of metal (mainly ferrous metals) and anticorrosion mechanism, the experimental results demonstrates polyaniline compound protective system compared with conventional protective system, and antiseptic property has had significant raising.
The factor affecting polyaniline anticorrosion is a lot, as: the content of oxygen and the surface treatment etc. of matrix in polyaniline structure, corrosive environment, coating system and corrosive medium.Its main application fields comprises: boats and ships, port and pier equipment, ocean containers. warship, amphibious plate armour, chemical industry equipment, high voltage iron tower, the weather resistance such as transmitting and transforming equipment, railroad bridge impregnating material.
The various experimental performance parameters of powder coating of the present invention:
(1) functional experiment of self-regeneration:
In powder coating of the present invention, polyaniline can be formed fine and close metal oxide layer and stops metal to corrode further in oxidized metal.Can also transmit the oxidizing mediums such as oxygen constantly arrives metallic surface to this functional materials simultaneously, the dense coating of formation is constantly increased, until hold together.Therefore, even coating defectiveness or scuffing, part metals expose, this tight zone just to where developing, until repair completely.Therefore, this coating has the function of self-regeneration, asks for an interview Fig. 1 (low frequency, the preservative effect of the higher coating of resistance when namely X-coordinate is-1 is better), as can be seen from Figure 1: common coating after 3 days common coating start to corrode appearance a little, still fine containing polyaniline coating impedance; After 12 days, common coating is by thorough corrosion failure, better containing polyaniline coating; 15 days post-dryings, good containing polyaniline coating self-regeneration, common coating cannot be repaired.
(2) salt leaching experiment: salt leaching experiment is exactly tests in the high temperature salt solution of testing plate being inserted ventilation, object be simulation under operating mode coating to the protective capacities of metal.
The condition that this experiment uses is: will coating testing plate be had to insert in the salt solution of the blowing air of 75 DEG C, separated in time, takes out and measures resistance value.Then, then insert, take out after certain hour and survey again.Result shows, coating has excellent antiseptic property, and in the immersion process of 20 days, none damages (being at least equivalent to salt-fog test 15000 hours) to coating.
Claims (3)
1. there is a Polyaniline powder paint for acid resistance self-repair function, it is characterized in that: its raw material forms component and parts by weight are respectively:
Described solidifying agent is imidazoles or phenols curing agent;
Described color stuffing is the mixture of one or more in common Rutile type Titanium Dioxide, carbon black, silicon powder or process white;
The mixture that described special epoxy resin forms for modified bisphenol A type epoxy resin, bisphenol A-type high molecular solid epoxy and o-cresol formaldehyde epoxy resin, modified bisphenol A type epoxy resin: bisphenol A-type high molecular solid epoxy: the mass ratio of o-cresol formaldehyde epoxy resin is: 280 ~ 320:130 ~ 180:30 ~ 50;
The described preparation method with the Polyaniline powder paint of acid resistance self-repair function, step is as follows:
(1) the preparation of polyaniline:
1. emulsion polymerization synthesized polyaniline technique: in the reactor in aniline: the ratio of the amount of substance of dodecylbenzene is that the ratio of 2:1 adds aniline and dodecylbenzene, water, dimethylbenzene is added successively after mixing, abundant stirring, to obtaining transparent emulsion;
2. then in transparent emulsion in ammonium persulphate: the ratio of the amount of substance of aniline is that the ratio of 1:1 drips ammonium persulphate (NH
4)
2s
2o
8the aqueous solution, system color slowly deepens, and keeps system temperature 0 ~ 20 DEG C, continues stirring 30 minutes, after during static storing 24, then adds acetone breakdown of emulsion, with ethanol or acetone repetitive scrubbing 3 ~ 4 times, removes ethanol or acetone, filters and to obtain precipitation;
3. use water, dodecylbenzenesulfonic acid solution washing precipitation substantially colourless to filtrate successively, vacuum-drying 48h at 40 DEG C, obtain the polyaniline powder adulterated;
(2) the preparation of powder coating:
By step (1) in the polyaniline powder of synthesis and special epoxy resin, solidifying agent, auxiliary agent, color stuffing press formula rate and weigh accurately, stir, extrude extrusion temperature 80 ~ 90 DEG C through twin screw extruder again, compressing tablet, Crushing of Ultrafine, to sieve, the Polyaniline powder paint of acid resistance self-repair function must be had.
2. powder coating according to claim 1, is characterized in that: described modified bisphenol A type epoxy resin: bisphenol A-type high molecular solid epoxy: the mass ratio of o-cresol formaldehyde epoxy resin is 300:150:35.
3. powder coating according to claim 1, is characterized in that: described polyaniline molecule structural formula is:
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| CN104893494B (en) * | 2015-05-13 | 2017-09-29 | 国润恒科（天津）防腐工程技术有限公司 | A kind of high bond stress of heavy antisepsis is double to apply thin layer reinforcing bar powdery paints and the reinforcing bar and preparation method and the application of the reinforcing bar |
| EP3388462A1 (en) | 2017-04-12 | 2018-10-17 | TIGER Coatings GmbH & Co. KG | Powder coating composition |
| CN107141967A (en) * | 2017-06-26 | 2017-09-08 | 浙江工业大学 | A kind of powdery paints of graphene-containing/polyaniline compounded mix and preparation method thereof |
| CN109535945A (en) * | 2018-12-21 | 2019-03-29 | 六安科瑞达新型材料有限公司 | A kind of open air salt spray resistance powdery paints |
| CN115613019A (en) * | 2022-09-29 | 2023-01-17 | 南京科润工业介质股份有限公司 | Waste heat blackening liquid for workpiece suitable for full-automatic weighing and packaging machine subpackaging |
| CN115584188B (en) * | 2022-12-14 | 2023-04-11 | 佛山市涂亿装饰材料科技有限公司 | Preparation method of powder coating and marbleized powder spraying coating |
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| CN1583830A (en) * | 2004-05-27 | 2005-02-23 | 西北核技术研究所 | Method for direct preparation of polyaniline solution from aniline monomer |
| CN1639278A (en) * | 2002-07-03 | 2005-07-13 | Ad技术株式会社 | Anti-corrosion paint for steel with polyaniline |
| CN102408813A (en) * | 2011-09-28 | 2012-04-11 | 国润恒科（天津）防腐工程技术有限公司 | High-electric-conductivity heavy-anticorrosion wave-absorbing powder paint |
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| US5532025A (en) * | 1993-07-23 | 1996-07-02 | Kinlen; Patrick J. | Corrosion inhibiting compositions |
| CN1639278A (en) * | 2002-07-03 | 2005-07-13 | Ad技术株式会社 | Anti-corrosion paint for steel with polyaniline |
| CN1583830A (en) * | 2004-05-27 | 2005-02-23 | 西北核技术研究所 | Method for direct preparation of polyaniline solution from aniline monomer |
| CN102408813A (en) * | 2011-09-28 | 2012-04-11 | 国润恒科（天津）防腐工程技术有限公司 | High-electric-conductivity heavy-anticorrosion wave-absorbing powder paint |
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