CN103992675A - Marine heavy-duty anti-corrosion coating and preparation method thereof - Google Patents
Marine heavy-duty anti-corrosion coating and preparation method thereof Download PDFInfo
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- CN103992675A CN103992675A CN201410249316.4A CN201410249316A CN103992675A CN 103992675 A CN103992675 A CN 103992675A CN 201410249316 A CN201410249316 A CN 201410249316A CN 103992675 A CN103992675 A CN 103992675A
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Abstract
The invention discloses a marine heavy-duty anti-corrosion coating and a preparation method thereof. The coating comprises the following components in parts by weight: 5-15 parts of mica powder, 10-15 parts of B-N ligand polyaniline/montmorillonite composite conductive material, 8-15 parts of talcum powder, 10-15 parts of quartz powder, 30-40 parts of matrix resin, 0-3 parts of pigment, 0.5-1.0 part of defoamer, 0.5-1.0 part of dispersant, 0.5-1.0 part of coalescing agents and 30-40 parts of solvent, wherein the B-N ligand polyaniline/montmorillonite composite conductive material is synthesized by montmorillonite activated and modified by a surfactant, an organic boronic acid, an aniline monomer and double phenolic hydroxyl derivatives; the organic boronic acid is one of a 2-methyl phenyl boronic acid, a 3-methyl phenyl boronic acid, a 4-methyl phenyl boronic acid, a 3,5-dimethylphenylboronic acid, a phenylboronic acid and 4-methoxy benzene boron; the double phenolic hydroxyl derivatives are one of 3,4-gentisic acid methyl ester, 3,4-dihydroxy benzaldehyde and 3,4-dihydroxy benzoic acid ethyl ester. The coating is excellent in corrosion resistance.
Description
Technical field
The invention belongs to heavy-duty coating technical field, relate to a kind of Marine Gravity And anticorrosive coating and preparation method thereof.
Background technology
Along with the fast development of China's marine economy, the market scale of Marine Paints product constantly expands, and the demand average annual growth rate of Marine Paints surpasses 20%.Except boats and ships and freight container, the ocean exploitation Infrastructure such as bridge spanning the sea all need to have the long anticorrosion time limit.Ocean protection against corrosion is one of gordian technique of oceanographic engineering, metal corrodes the stress corrosion fracture (SCC) that causes, hydrogen embrittlement (HE), corrosion fatigue (CF), intergranular corrosion (IC) etc. in ocean can make oceanographic engineering steel construction that fracture suddenly occurs, cause ocean environment eco-catastrophe, bring about great losses.In addition, the idle cost that the inefficacy in advance of oceanographic engineering product corrosion protection coating and coating maintenance bring is also quite large, traditional antifouling anticorrosive coating utilizes the toxicants such as Red copper oxide or tin class suppress adhering to of marine life and grow, but these toxicants have caused severe contamination to seawater.Therefore, find the direction that novel antifouling anticorrosive coating nontoxic, high Corrosion Protection has become people's research.
In recent years, polyaniline is taken seriously gradually as a kind of good impregnating material.Yet, because polyaniline is insoluble not molten, limited its widespread use technically.Existing polyaniline anticorrosion paint mainly contains following two kinds: (1) electrochemistry forms polyaniline coating, but this method is difficult to be applied to the anti-corrosive treatment of site operation and large-scale metal parts, is not also suitable for industrialization and produces.(2) polyaniline and conventional film-forming resin blend are prepared into composite coating, the method has overcome the deficiency of electrochemical polymerization, be at present main research field, but the addition of required polyaniline is higher, and economic benefit has much room for improvement.
For improving ability and the processing characteristics of the polyaniline paint medium of resistance to strong corrosion, polyaniline is composite modified is the method for a practical and applicable suitability for industrialized production.Intercalation polymeric is one of effective ways of preparing high performance composite, is about to polyalcohol intercalation in the silicate of laminate structure, as vermiculite, mica, polynite etc.Polynite (MMT) is comprised of the thick silicate lamella of 1nm, lamella is comprised of silicon-oxy tetrahedron and alumina octahedral, interlayer maintains balance by Liquidity limit conventionally, because polynite is a kind of inertia main body without oxidizing property, thereby be inserted into interlayer monomer polymerization as required manual control monomer is inserted between stratiform lamella or space, and then the laminated structure of destruction silicate, it is peeled off becomes nanoscale twins and is evenly dispersed in polymeric matrix, to realize compound at nano-scale of polymer and clay class silicate, thereby obtain being different from the premium properties of general matrix material.
At present, about the research of the preparation of polynite and polyaniline composite material and conduction Corrosion Protection thereof, there are reports.(the method for preparing the intercalated nano-composite of polyaniline or polyaniline derivative and inorganic clay by mechanochemistry polymerization such as Zheng Hao; Chinese patent; publication number CN 103265698 A) disclose and a kind ofly under argon shield, used mechanochemistry polymerization to prepare the method for intercalated nano-composite polyaniline and polyaniline derivative, inorganic clay, obtained having the matrix material of good dispersion and physical strength.But its preparation process need to vacuumize and nitrogen protection repeatedly, is not suitable for suitability for industrialized production, thereby its scale operation is restricted.(the aqueous polyanion metal composite anti-corrosion material and preparation method thereof such as Wang Yunpu, Chinese patent, publication number CN 1803951 A) disclose a kind of aqueous polyanion composite anticorrosion coating that sodium-based montmorillonite, aniline, aqueous epoxy resin emulsion, polystyrolsulfon acid, ammonium persulphate etc. are prepared as main raw material of take, there is the advantages such as cost is low, environmental pollution is little.But be difficult to better realize the dispersion of polyaniline and polynite, only obtain simple physical blending, can not bring into play the advantage of each component maximum of matrix material.(polyaniline composite material and the preparation method that the clay mineral of take is carrier such as Ye Ying, Chinese patent, publication number CN 1381530 A) a kind of electrically conductive polyaniline through protonic acid doping (PANI) in-situ polymerization is disclosed, be coated on polyaniline composite material and preparation method on clay mineral, had the good physical and chemical performance of polyaniline and clay concurrently.But matrix material prepared by this method has only been realized macroscopical physical blending, and can not make polyaniline enter between the lamella of polynite, reach the compatible of nanoscale, thereby the performance of material is not greatly improved.
Summary of the invention
Object of the present invention is intended to overcome prior art defect, and a kind of Marine Gravity And anticorrosive coating is provided.
Another object of the present invention is to provide the preparation method of above-mentioned Marine Gravity And anticorrosive coating.
Technical scheme of the present invention is as follows:
A Marine Gravity And anticorrosive coating, is comprised of the component of following weight part proportioning:
Described B-N polycomplexation aniline and montmorillonite composite material are synthetic by polynite, organic boronic, aniline monomer and two Hydroxyphenol derivatives of ionic surface active agent activation modification, wherein said organic boronic is 2-methylphenylboronic acid, 3-methylphenylboronic acid, 4-methylphenylboronic acid, 3, a kind of in 5-dimethylphenyl boronic acid, phenylo boric acid and 4-anisole boron, concrete structure is as follows:
Described organic boronic can be a kind of of following compound:
Described pair of Hydroxyphenol derivatives is MDB, 3, a kind of in 4-Dihydroxy benzaldehyde and PCA ethyl ester.
In a preferred embodiment of the invention, the described polynite by ionic surface active agent activation modification is organo montmorillonite a kind of of CTAB, CTAC modification, the organo montmorillonite of producing as Zhejiang Feng Hong clay Chemical Co., Ltd..
In a preferred embodiment of the invention, the fineness of described mica powder, talcum powder and silica powder is 800～1000 orders.
In a preferred embodiment of the invention, described matrix resin is a kind of in epoxy resin, fluorocarbon resin, urethane resin, aminoresin, acrylic resin, Synolac, vibrin.
In a preferred embodiment of the invention, described pigment is a kind of in titanium dioxide, carbon black, red iron oxide, ultramarine, Lemon chrome yellow.
In a preferred embodiment of the invention, described solvent is at least one in BDDE, ethylene glycol diglycidylether, acetone, dimethylbenzene, propyl carbinol, methyl iso-butyl ketone (MIBK), dehydrated alcohol, vinyl acetic monomer, N-BUTYL ACETATE.
In a preferred embodiment of the invention, described defoamer is a kind of in silicone based defoamer, inorganic silicon defoamer and antifoaming agent of non-silicone, a kind of in the Efka2018 that BYK302, BYK065, BYK20, BYK011, BYK053 or the EFKA company producing as German Bi Ke company produces.
In a preferred embodiment of the invention, described dispersion agent is solvent-borne type dispersion agent or wetting dispersing agent, BYK101, the BYK161, the BYK163 that produce as German Bi Ke company, or the Efka5044 that produces of EFKA company.
In a preferred embodiment of the invention, described film coalescence aid is a kind of in butyl Bian alcohol acetic ester, butyl glycol ether carboxylic ester, ethylene glycol phenyl ether, dibasic acid dimethyl ester, propylene glycol propyl ether, diprotic acid diethyl ester class.
A preparation method for above-mentioned Heavy-duty Coatings In Ocean Chemical Industry, comprises the steps:
(1) prepare B-N polycomplexation aniline/montmorillonite Composite electro-conductive material, comprise the steps:
A, the polynite by ionic surface active agent activation modification is added in the organic boronic solution of 1mol/L of 10 times of weight parts and disperses, at room temperature the speed with 600～1000r/min stirs 4～6h, form suspension system, by accounting for aniline monomer by the polynite weight 16～20% of ionic surface active agent activation modification, join above-mentioned suspension system and carry out the in-situ inserted reaction of aniline again, continue to stir 4～6h and make intercalation abundant, obtain aniline emulsion;
Under b, room temperature, by adding in described aniline emulsion with the oxygenant of molar weight, two Hydroxyphenol derivatives of 10～30% of accounting for by the polynite weight of ionic surface active agent activation modification with aniline monomer, under nitrogen protection, reaction 6～8h;
C, reaction finish rear elder generation and in water, carry out ultrasonic dispersion, then carry out centrifugation, and it is neutral that the precipitate with deionized water of gained, acetone repetitive scrubbing to filtrate are, and gained precipitation is dry, through grinding, obtain B-N polycomplexation aniline/montmorillonite Composite electro-conductive material;
(2) prepare Marine Gravity And anticorrosive coating: each component is fully mixed and disperses 1～4h, after filtration, obtain Marine Gravity And anticorrosive coating.
In a preferred embodiment of the invention, described oxygenant is ammonium persulphate ((NH
4)
2s
2o
8), Potassium Persulphate (K
2s
2o
8), iron trichloride (FeCl
3) or ferric sulfate (Fe
2(SO
4)
3);
The invention has the beneficial effects as follows: first the present invention utilizes organic boronic and organo montmorillonite mix and blend, organic boronic can activate aniline as dopant acid solution can increase interlamellar spacing with the N coordination of polynite by ionic surface active agent activation modification again, because B element after B-N coordination is by flush type SP
2hybrid structure is converted to three-dimensional SP
3hybrid structure, making N between montmorillonite layer and organic boronic coordination support the intercalation polymeric that large montmorillonite layer spacing is conducive to aniline reacts, organic boronic can serve as the effect activation aniline of proton dopant acid simultaneously, later stage is in the polymerization process of aniline, the two Hydroxyphenol derivatives that add and the part boric acid of organo montmorillonite interlayer are condensed into boric acid ester and are beneficial to the coordination with polyaniline, realize supramolecular structure, form the electric conductivity that larger conjugated system is conducive to polymkeric substance simultaneously, improve the anti-corrosion of metal performance of conducting polyaniline composite material;
Accompanying drawing explanation
Fig. 1 is the coordination process schematic diagram of the step a of the embodiment of the present invention 1 step (1);
Fig. 2 is organic boronic and by the nucleus magnetic resonance boron spectrogram before the N ligand complex of cetyl trimethylammonium bromide (CTAB) between the cheating engaging layer of ionic surface active agent activation modification, X-coordinate is chemical shift Chemical shift (ppm) in the embodiment of the present invention 2 steps (1).
Fig. 3 is organic boronic and by the nucleus magnetic resonance boron spectrogram after the N ligand complex of cetyl trimethylammonium bromide (CTAB) between the cheating engaging layer of ionic surface active agent activation modification, X-coordinate is chemical shift Chemical shift (ppm) in the embodiment of the present invention 2 steps (1).
Fig. 4 is B-N polycomplexation aniline/montmorillonite Composite electro-conductive material of preparation in the embodiment of the present invention 2 steps (1), by the XRD diffractogram of the polynite of ionic surface active agent activation modification, X-coordinate be diffraction angle 2 θ (°), ordinate zou is the intensity (a.u.) at peak, curve a is B-N polycomplexation aniline/montmorillonite Composite electro-conductive material prepared by the present embodiment, and curve b is the polynite by ionic surface active agent activation modification.
Fig. 5 is that the magnification of B-N polycomplexation aniline/montmorillonite Composite electro-conductive material of preparation in embodiment 2 steps (1) is the stereoscan photograph of 20000 times, and scale is 400nm.
Fig. 6 is that the magnification of B-N polycomplexation aniline/montmorillonite Composite electro-conductive material of preparation in embodiment 3 steps (1) is the stereoscan photograph of 11000 times, and scale is 400nm.
Embodiment
By embodiment, technical scheme of the present invention is further detailed and is described below.
In following each embodiment:
The described polynite by ionic surface active agent activation modification is organo montmorillonite a kind of of CTAB, CTAC modification, the organo montmorillonite of producing as Zhejiang Feng Hong clay Chemical Co., Ltd..
Described organic boronic is 2-methylphenylboronic acid, 3-methylphenylboronic acid, 4-methylphenylboronic acid, 3, a kind of in 5-dimethylphenyl boronic acid, phenylo boric acid and 4-anisole boron;
Described pair of Hydroxyphenol derivatives is MDB, 3, a kind of in 4-Dihydroxy benzaldehyde and PCA ethyl ester.
The fineness of described mica powder, talcum powder and silica powder is 800～1000 orders.
Described matrix resin is a kind of in epoxy resin, fluorocarbon resin, urethane resin, aminoresin, acrylic resin, Synolac and vibrin.
Described pigment is a kind of in titanium dioxide, carbon black, red iron oxide, ultramarine and Lemon chrome yellow.
Described solvent is at least one in BDDE, ethylene glycol diglycidylether, acetone, dimethylbenzene, propyl carbinol, methyl iso-butyl ketone (MIBK), dehydrated alcohol, vinyl acetic monomer, N-BUTYL ACETATE.
Described defoamer is a kind of in silicone based defoamer, inorganic silicon defoamer and antifoaming agent of non-silicone.
Described dispersion agent is solvent-borne type dispersion agent or wetting dispersing agent.
Described film coalescence aid is a kind of in butyl Bian alcohol acetic ester, butyl glycol ether carboxylic ester, ethylene glycol phenyl ether, dibasic acid dimethyl ester, propylene glycol propyl ether and diprotic acid diethyl ester class.
Described oxygenant is a kind of in ammonium persulphate, Potassium Persulphate, iron trichloride and ferric sulfate.
Embodiment 1
(1) preparation of B-N polycomplexation aniline/montmorillonite Composite electro-conductive material
A, the CTAB organic modification montmonrillonite of 50 parts is added in the organic boronic solution of 1mol/L of 500 parts and disperses, at room temperature through stirrer, the speed with 800r/min stirs, form suspension system, continue to stir 5h, the aniline monomer of 10 parts is joined to suspension and carry out the in-situ inserted reaction of aniline, continue to stir 6h and make intercalation abundant, the coordination process of this step as shown in Figure 1;
B, at room temperature, by adding in described aniline emulsion with the oxygenant of molar weight, 10 parts of two Hydroxyphenol derivatives with aniline monomer, under nitrogen protection, reaction 8h;
C, reaction finish rear elder generation and in water, carry out ultrasonic dispersion, then carry out centrifugation, and it is neutral that the precipitate with deionized water of gained, acetone repetitive scrubbing to filtrate are, and gained precipitation is dry, through grinding, obtain polyaniline and montmorillonite Composite conducting material powder;
(2) preparation of described Marine Gravity And anticorrosive coating
By the component proportioning of heavy duty system, get 15 parts of B-N polycomplexation aniline/montmorillonite composite materials, 10 parts of mica powders, 10 parts of talcum powder, 15 parts of silica powders, 30 parts of matrix resins, 2 parts of pigment, 0.50 part of defoamer, 0.50 part of dispersion agent, 0.50 part of film coalescence aid, 30 parts of solvent, dispersed 4h on dispersion machine, after filtration, can obtain Marine Gravity And anticorrosive coating, its antiseptic property test result is as shown in table 1.
Embodiment 2
(1) preparation of B-N polycomplexation aniline/montmorillonite Composite electro-conductive material
A, the CTAB organic modification montmonrillonite of 50 parts is added in the organic boronic solution of 1mol/L of 500 parts and disperses, at room temperature through stirrer, the speed with 700r/min stirs, form suspension system, continue to stir 5h, the aniline monomer of 12 parts is joined to suspension and carry out the in-situ inserted reaction of aniline, continue to stir 6h and make intercalation abundant;
B, at room temperature, by adding in described aniline emulsion with the oxygenant of molar weight, 15 parts of two Hydroxyphenol derivatives with aniline monomer, under nitrogen protection, reaction 8h;
C, reaction finish rear elder generation and in water, carry out ultrasonic dispersion, carry out again centrifugation, it is neutral that the precipitate with deionized water of gained, acetone repetitive scrubbing to filtrate are, and gained precipitation is dry, through grinding, obtains polyaniline and montmorillonite Composite conducting material powder (as shown in Figures 2 to 5);
(2) preparation of described Marine Gravity And anticorrosive coating
By the component proportioning of heavy duty system, get 10 parts of B-N polycomplexation aniline/montmorillonite composite materials, 10 parts of mica powders, 15 parts of talcum powder, 10 parts of silica powders, 35 parts of matrix resins, 2 parts of pigment, 0.70 part of defoamer, 0.70 part of dispersion agent, 0.70 part of film coalescence aid, 30 parts of solvent, dispersed 4h on dispersion machine, after filtration, can obtain Marine Gravity And anticorrosive coating, its antiseptic property test result is as shown in table 1.
Embodiment 3
(1) preparation of B-N polycomplexation aniline/montmorillonite Composite electro-conductive material
A, the CTAB organic modification montmonrillonite of 50 parts is added in the organic boronic solution of 1mol/L of 500 parts and disperses, at room temperature through stirrer, the speed with 1000r/min stirs, form suspension system, continue to stir 5h, the aniline monomer of 15 parts is joined to suspension and carry out the in-situ inserted reaction of aniline, continue to stir 6h and make intercalation abundant;
B, at room temperature, by adding in described aniline emulsion with the oxygenant of molar weight, 5 parts of two Hydroxyphenol derivatives with aniline monomer, under nitrogen protection, reaction 8h;
C, reaction finish rear elder generation and in water, carry out ultrasonic dispersion, carry out again centrifugation, it is neutral that the precipitate with deionized water of gained, acetone repetitive scrubbing to filtrate are, and gained precipitation is dry, through grinding, obtains polyaniline and montmorillonite Composite conducting material powder (as shown in Figure 6);
(2) preparation of described Marine Gravity And anticorrosive coating is got 15 parts of B-N polycomplexation aniline/montmorillonite composite materials, 10 parts of mica powders, 15 parts of talcum powder, 10 parts of silica powders, 40 parts of matrix resins, 2 parts of pigment, 1.0 parts of defoamers, 1.0 parts of dispersion agents, 1.0 parts of film coalescence aid, 30 parts of solvent by the component proportioning of heavy duty system, dispersed 4h on dispersion machine, after filtration, can obtain Marine Gravity And anticorrosive coating, its antiseptic property test result is as shown in table 1.
The antiseptic property test result of the Marine Gravity And anticorrosive coating of table 1 embodiment 1 to 3
The above, be only preferred embodiment of the present invention, therefore can not limit according to this scope of the invention process, the equivalence done according to the scope of the claims of the present invention and description changes and modifies, and all should still belong in the scope that the present invention contains.
Claims (10)
1. a Marine Gravity And anticorrosive coating, is characterized in that: the component by following weight part proportioning forms:
Wherein said B-N polycomplexation aniline/montmorillonite Composite electro-conductive material is synthetic by polynite, organic boronic, aniline monomer and two Hydroxyphenol derivatives of ionic surface active agent activation modification, wherein said organic boronic is 2-methylphenylboronic acid, 3-methylphenylboronic acid, 4-methylphenylboronic acid, 3, a kind of in 5-dimethylphenyl boronic acid, phenylo boric acid and 4-anisole boron; Described pair of Hydroxyphenol derivatives is MDB, 3, a kind of in 4-Dihydroxy benzaldehyde and PCA ethyl ester.
2. a kind of Marine Gravity And anticorrosive coating as claimed in claim 1, is characterized in that: the fineness of described mica powder, talcum powder and silica powder is 800～1000 orders.
3. a kind of Marine Gravity And anticorrosive coating as claimed in claim 1, is characterized in that: described matrix resin is a kind of in epoxy resin, fluorocarbon resin, urethane resin, aminoresin, acrylic resin, Synolac and vibrin.
4. a kind of Marine Gravity And anticorrosive coating as claimed in claim 1, is characterized in that: described pigment is a kind of in titanium dioxide, carbon black, red iron oxide, ultramarine and Lemon chrome yellow.
5. a kind of Marine Gravity And anticorrosive coating as claimed in claim 1, it is characterized in that: described solvent is at least one in BDDE, ethylene glycol diglycidylether, acetone, dimethylbenzene, propyl carbinol, methyl iso-butyl ketone (MIBK), dehydrated alcohol, vinyl acetic monomer, N-BUTYL ACETATE.
6. a kind of Marine Gravity And anticorrosive coating as claimed in claim 1, is characterized in that: described defoamer is a kind of in silicone based defoamer, inorganic silicon defoamer and antifoaming agent of non-silicone.
7. a kind of Marine Gravity And anticorrosive coating as claimed in claim 1, is characterized in that: described dispersion agent is solvent-borne type dispersion agent or wetting dispersing agent.
8. a kind of Marine Gravity And anticorrosive coating as claimed in claim 1, is characterized in that: described film coalescence aid is a kind of in butyl Bian alcohol acetic ester, butyl glycol ether carboxylic ester, ethylene glycol phenyl ether, dibasic acid dimethyl ester, propylene glycol propyl ether and diprotic acid diethyl ester class.
9. by a preparation method for the Marine Gravity And anticorrosive coating described in arbitrary claim in claim 1 to 8, it is characterized in that: comprise the steps:
(1) prepare B-N polycomplexation aniline/montmorillonite Composite electro-conductive material, comprise the steps:
A, the polynite by ionic surface active agent activation modification is joined in the organic boronic solution of 1mol/L of ten times of weight parts and disperse, at room temperature the speed with 600～1000r/min stirs 4～6h, form suspension system, by accounting for aniline monomer by the polynite weight 16～20% of ionic surface active agent activation modification, add and in above-mentioned suspension system, carry out the in-situ inserted reaction of aniline again, continue to stir 4～6h and make intercalation abundant, obtain aniline emulsion;
Under b, room temperature, by adding in described aniline emulsion with the oxygenant of molar weight, two Hydroxyphenol derivatives of 10～30% of accounting for by the polynite weight of ionic surface active agent activation modification with aniline monomer, under nitrogen protection, reaction 6～8h;
C, reaction finish rear elder generation and in water, carry out ultrasonic dispersion, then carry out centrifugation, and it is neutral that the precipitate with deionized water of gained, acetone repetitive scrubbing to filtrate are, and gained precipitation is dry, through grinding, obtain B-N polycomplexation aniline/montmorillonite Composite electro-conductive material;
(2) prepare Marine Gravity And anticorrosive coating: each component is fully mixed and disperses 1～4h, after filtration, obtain Marine Gravity And anticorrosive coating.
10. preparation method as claimed in claim 9, is characterized in that: described oxygenant is a kind of in ammonium persulphate, Potassium Persulphate, iron trichloride and ferric sulfate.
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| CN104313591A (en) * | 2014-11-07 | 2015-01-28 | 合肥大安印刷有限责任公司 | Long-acting water-based antirust agent and preparation method thereof |
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