CN107177280B - A kind of carbonation corrosion-resistant epoxy paint and preparation method thereof - Google Patents
A kind of carbonation corrosion-resistant epoxy paint and preparation method thereof Download PDFInfo
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- CN107177280B CN107177280B CN201710392034.3A CN201710392034A CN107177280B CN 107177280 B CN107177280 B CN 107177280B CN 201710392034 A CN201710392034 A CN 201710392034A CN 107177280 B CN107177280 B CN 107177280B
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/08—Anti-corrosive paints
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Abstract
The invention discloses a kind of carbonation corrosion-resistant epoxy paint and preparation method thereof, silica and pyrrole monomer are carried out amidatioon crosslinking by the coating of the present invention, then it polymerize again, the compatibility between silica and polymer can be strengthened, improve the stability_intensity of finished product film, the silica added simultaneously can also improve the toughness of finished product film, case hardness and impact strength, the polypyrrole coating of the present invention can form the oxide-film of a floor height consistency in metallic substrate surface, enhance it and suppress the ability of anode reaction, preferably isolating metal base material and corrosive medium, show more preferable corrosion resistance, successfully corrosion of the corrosive medium to low-carbon steel material is delayed.
Description
Technical field
The invention belongs to composite material paint field, and in particular to a kind of carbonation corrosion-resistant epoxy paint and its preparation
Method.
Background technology
The metal that there are conducting polymer composite coating conventional coatings to hang back is passivated and anodic protection function, while simultaneous
Standby anti scuffing acts on, and anti-corrosion material certainly will turn into one of conducting polymer prospect of the application category the brightest, conducting polymer
By compound with other materials, composite coating is set to reach ageing-resistant, acid and alkali-resistance, the technical indicator of good mechanical performance；
Compared with solvent based coating, water paint has many advantages, such as, as VOC content is low, smell is low, it is nonflammable, make
With safely, can wash by water.Therefore epoxy resin is carried out Water-borne modification processing by people, water paint is made, to meet more
High requirement.The research and development of many decades and application practice prove that water-base epoxy paint coating has adhered to many excellent of epoxy resin
Point, excellent to the adhesive force of steel, cement, shrinkage factor is low, there is good corrosion resistance and impervious to intermediate acid, alkali and other solvents
Permeability, it can be configured to a series of conventional anti-corrosive paints with good miscible of various resins, filler and auxiliary agent, one can be formed
The system of water corrosion-resistant epoxy paint；
But compared with solvent based coating, the formula of water paint is complicated, a variety of inorganic additives have been generally comprised, and these
Inorganic additive because of the bad dispersibility with resin, can have influence on the stability of film, cause the hydraulic performance decline of film
The content of the invention
It is an object of the invention to the bad dispersibility of the middle inorganic additive and resin for prior art, film is caused
A kind of the problem of stability difference, there is provided carbonation corrosion-resistant epoxy paint and preparation method thereof.
To achieve the above object, the present invention uses following technical scheme：
A kind of carbonation corrosion-resistant epoxy paint and preparation method thereof, comprises the following steps：
(1) maleic anhydride of 2-3 parts by weight is taken, is added in the deionized water of 30-40 times of its weight, stirs, add
Enter the zinc acetylacetonate of 0.1-0.2 parts by weight, increase the temperature to 60-70 DEG C, insulated and stirred 5-10 minutes, obtain acidification hydrolization liquid；
(2) pyrroles of 160-170 parts by weight is taken, is added in the tetrahydrofuran of 30-44 times of its weight, stirs, send
Enter into 60-70 DEG C of water bath with thermostatic control, add the metallic potassium of 1-2 parts by weight, insulated and stirred 30-40 minutes, discharging cooling, add
The paratoluensulfonyl chloride of 5-7 parts by weight, magnetic agitation 20-24 hours, product is added in deionized water, stirred, it is quiet
Put 10-15 hours, filter, sediment is washed, 1-2 hours are dried at 60-70 DEG C of vacuum, obtain sulphonylpyrroles；
(3) carbonic acid of 5-6 parts by weight is taken, is added in the deionized water of 20-30 times of its weight, stirs；
(4) above-mentioned acidification hydrolization liquid is taken, mixes, stirs with sulphonylpyrroles, ultrasonic 10-20 minutes, adds 0.3-1
Alkanolamide, the silica of 13-15 parts by weight of parts by weight, stir, and obtain acid amides pyrroles's dispersion liquid；
(5) phenol of 10-15 parts by weight is taken, heating melting is added dropwise above-mentioned carbonate aqueous solution, insulated and stirred 10-20 minutes,
Sodium hydroxide is added, regulation pH is 7-8, stirring reaction 1-2 hours, obtains carbonization ester solution；
(6) above-mentioned acid amides pyrroles dispersion liquid, carbonization ester solution are mixed, stirs, be sent in reactor, be passed through nitrogen
Gas, regulation temperature of reaction kettle are 4-6 DEG C, insulation reaction 4-5 hours, discharge, filtering, sediment are washed, vacuum 70-75
20-23 hours are dried at DEG C, is added in the deionized water of 100-110 times of its weight, ultrasonic 10-15 minutes, obtains silica
Modified polypyrrole solution；
(7) epoxy resin of 130-140 parts by weight is taken, is mixed with silica modified polypyrrole solution, 4000-5000
Turn/part stirring 1-2 hours, obtain carbonation corrosion-resistant epoxy paint.
The application method of coating of the present invention is：Take the coating of the present invention, the methyl hexahydro neighbour benzene two with its weight 15-30%
Formic anhydride mixes, and stirs, is coated to metallic substrate surface, the heat preservation solidification 100-150 minutes at 100-130 DEG C, you can.
The invention has the advantages that the present invention hydrolyzes to obtain acid solution first by maleic anhydride, then by pyrroles
Sulfonylation is carried out by paratoluensulfonyl chloride, then mixed with hydrolyzing obtained acid solution, amidatioon crosslinking is carried out, incites somebody to action afterwards
The cross-linking products arrived mix with silica, are disperseed by alkanolamide, are finally polymerize acid amides pyrroles's dispersion liquid,
It is distributed to again with epoxy blend in deionized water, obtains water-based anticorrosive paint；
Silica and pyrrole monomer are carried out amidatioon crosslinking by the coating of the present invention, are then polymerize again, can be strengthened two
Compatibility between silica and polymer, the stability_intensity of finished product film is improved, while the silica added can also carry
Toughness, case hardness and the impact strength of high finished product film, polypyrrole epoxy coating of the invention can be in metal base tables
Face forms the oxide-film of a floor height consistency, enhances it and suppresses the ability of anode reaction, preferably isolating metal base material and corruption
Medium is lost, more preferable corrosion resistance is shown, has successfully delayed corrosion of the corrosive medium to low-carbon steel material.
Embodiment
Embodiment 1
A kind of preparation method of carbonation corrosion-resistant epoxy paint, comprises the following steps：
(1) maleic anhydride of 2 parts by weight is taken, is added in the deionized water of 38 times of its weight, stirs, adds 0.1
The zinc acetylacetonate of parts by weight, 66 DEG C are increased the temperature to, insulated and stirred 9 minutes, obtains acidification hydrolization liquid；
(2) pyrroles of 165 parts by weight is taken, is added in the tetrahydrofuran of 38 times of its weight, stirs, be sent to 61 DEG C
Water bath with thermostatic control in, add 1 parts by weight metallic potassium, insulated and stirred 36 minutes, discharging cooling, add 5 parts by weight to toluene
Sulfonic acid chloride, magnetic agitation 20 hours, product is added in deionized water, stirred, and stands 14 hours, filtering, will be precipitated
Thing is washed, and is dried 1 hour at 60-70 DEG C of vacuum, is obtained sulphonylpyrroles；
(3) carbonic acid of 5 parts by weight is taken, is added in the deionized water of 21 times of its weight, stirs；
(4) above-mentioned acidification hydrolization liquid is taken, mixes, stirs with sulphonylpyrroles, ultrasound 17 minutes, adds 0.8 weight
The alkanolamide, the silica of 13 parts by weight of part, stir, obtain acid amides pyrroles's dispersion liquid；
(5) phenol of 14 parts by weight is taken, heating melting, above-mentioned carbonate aqueous solution is added dropwise, insulated and stirred 16 minutes, adds hydrogen
Sodium oxide molybdena, regulation pH is 7, stirring reaction 1 hour, obtains carbonization ester solution；
(6) above-mentioned acid amides pyrroles dispersion liquid, carbonization ester solution are mixed, stirs, be sent in reactor, be passed through nitrogen
Gas, regulation temperature of reaction kettle are 5 DEG C, insulation reaction 4 hours, discharge, filtering, sediment are washed, are done at 70 DEG C of vacuum
Dry 20 hours, it is added in the deionized water of 108 times of its weight, ultrasound 13 minutes, obtains silica modified polypyrrole solution；
(7) epoxy resin of 136 parts by weight is taken, is mixed with silica modified polypyrrole solution, 4000 turns/part stirring 1
Hour, obtain carbonation corrosion-resistant epoxy paint.
The application method of coating of the present invention is：
The coating of the present invention is taken, mixes, stirs with the methylhexahydrophthalic anhydride of its weight 20%, be coated to
Metallic substrate surface, heat preservation solidification 100 minutes at 110 DEG C, you can.
Embodiment 2
A kind of preparation method of carbonation corrosion-resistant epoxy paint, comprises the following steps：
(1) maleic anhydride of 3 parts by weight is taken, is added in the deionized water of 40 times of its weight, stirs, adds 0.2
The zinc acetylacetonate of parts by weight, 70 DEG C are increased the temperature to, insulated and stirred 10 minutes, obtains acidification hydrolization liquid；
(2) pyrroles of 170 parts by weight is taken, is added in the tetrahydrofuran of 44 times of its weight, stirs, be sent to 70 DEG C
Water bath with thermostatic control in, add 2 parts by weight metallic potassium, insulated and stirred 40 minutes, discharging cooling, add 7 parts by weight to toluene
Sulfonic acid chloride, magnetic agitation 24 hours, product is added in deionized water, stirred, and stands 15 hours, filtering, will be precipitated
Thing is washed, and is dried 2 hours at 60 DEG C of vacuum, is obtained sulphonylpyrroles；
(3) carbonic acid of 6 parts by weight is taken, is added in the deionized water of 30 times of its weight, stirs；
(4) above-mentioned acidification hydrolization liquid is taken, mixes, stirs with sulphonylpyrroles, ultrasound 20 minutes, adds 1 parts by weight
Alkanolamide, the silica of 15 parts by weight, stir, obtain acid amides pyrroles's dispersion liquid；
(5) phenol of 15 parts by weight is taken, heating melting, above-mentioned carbonate aqueous solution is added dropwise, insulated and stirred 20 minutes, adds hydrogen
Sodium oxide molybdena, regulation pH is 8, stirring reaction 2 hours, obtains carbonization ester solution；
(6) above-mentioned acid amides pyrroles dispersion liquid, carbonization ester solution are mixed, stirs, be sent in reactor, be passed through nitrogen
Gas, regulation temperature of reaction kettle are 6 DEG C, insulation reaction 5 hours, discharge, filtering, sediment are washed, are done at 75 DEG C of vacuum
Dry 23 hours, it is added in the deionized water of 110 times of its weight, ultrasound 15 minutes, obtains silica modified polypyrrole solution；
(7) epoxy resin of 140 parts by weight is taken, is mixed with silica modified polypyrrole solution, 5000 turns/part stirring 2
Hour, obtain carbonation corrosion-resistant epoxy paint.
The application method of coating of the present invention is：
The coating of the present invention is taken, mixes, stirs with the methylhexahydrophthalic anhydride of its weight 30%, be coated to
Metallic substrate surface, heat preservation solidification 150 minutes at 130 DEG C, you can.
Embodiment 3
A kind of preparation method of carbonation corrosion-resistant epoxy paint, comprises the following steps：
(1) maleic anhydride of 2 parts by weight is taken, is added in the deionized water of 30 times of its weight, stirs, adds 0.1
The zinc acetylacetonate of parts by weight, 60 DEG C are increased the temperature to, insulated and stirred 5 minutes, obtains acidification hydrolization liquid；
(2) pyrroles of 160 parts by weight is taken, is added in the tetrahydrofuran of 30 times of its weight, stirs, be sent to 60 DEG C
Water bath with thermostatic control in, add 1 parts by weight metallic potassium, insulated and stirred 30 minutes, discharging cooling, add 5 parts by weight to toluene
Sulfonic acid chloride, magnetic agitation 20 hours, product is added in deionized water, stirred, and stands 10 hours, filtering, will be precipitated
Thing is washed, and 1- hours are dried at 60 DEG C of vacuum, obtain sulphonylpyrroles；
(3) carbonic acid of 5 parts by weight is taken, is added in the deionized water of 20 times of its weight, stirs；
(4) above-mentioned acidification hydrolization liquid is taken, mixes, stirs with sulphonylpyrroles, ultrasound 10 minutes, adds 0.3 weight
The alkanolamide, the silica of 13 parts by weight of part, stir, obtain acid amides pyrroles's dispersion liquid；
(5) phenol of 10 parts by weight is taken, heating melting, above-mentioned carbonate aqueous solution is added dropwise, insulated and stirred 10 minutes, adds hydrogen
Sodium oxide molybdena, regulation pH is 7, stirring reaction 1 hour, obtains carbonization ester solution；
(6) above-mentioned acid amides pyrroles dispersion liquid, carbonization ester solution are mixed, stirs, be sent in reactor, be passed through nitrogen
Gas, regulation temperature of reaction kettle are 4 DEG C, insulation reaction 4 hours, discharge, filtering, sediment are washed, are done at 70 DEG C of vacuum
Dry 20 hours, it is added in the deionized water of 100 times of its weight, ultrasound 10 minutes, obtains silica modified polypyrrole solution；
(7) epoxy resin of 130 parts by weight is taken, is mixed with silica modified polypyrrole solution, 4000 turns/part stirring 1
Hour, obtain carbonation corrosion-resistant epoxy paint.
The application method of coating of the present invention is：Take the coating of the present invention, the methyl hexahydro O-phthalic with its weight 15%
Acid anhydrides mixes, and stirs, is coated to metallic substrate surface, heat preservation solidification 100 minutes at 100 DEG C, you can.
Performance test：
Sodium chloride of the paint film that the Esterification corrosion-resistant epoxy paint of the present invention is formed in metallic substrate surface in 3.5wt% is molten
Soaked 3 days in liquid, the shear strength for measuring paint film is 18-22MPa；Soaked 3 days in 10wt% hydrochloric acid solution, measure paint film
Shear strength be 19-23MPa；Soaked 3 days in 10wt% sodium hydroxide solution, the shear strength for measuring paint film is 19-
22MPa；
Comparative example：
Conventional epoxies coating is soaked in sodium chloride solution of the paint film that metallic substrate surface is formed in 3.5wt%
3 days, the shear strength for measuring paint film was 11-13MPa；Soaked 3 days in 10wt% hydrochloric acid solution, the shearing for measuring paint film is strong
Spend for 9-10MPa；Soaked 3 days in 10wt% sodium hydroxide solution, the shear strength for measuring paint film is 10-12MPa.
It can be seen that the paint film of the present invention has more preferable stability_intensity, to the corrosion protection of metal base more
By force.
It is complete by above-mentioned description, relevant staff using the above-mentioned desirable embodiment according to the present invention as enlightenment
Various changes and amendments can be carried out without departing from the scope of the technological thought of the present invention' entirely.The technology of this invention
Property scope is not limited to the content on specification, it is necessary to determines its technical scope according to right.
Claims (2)
1. a kind of preparation method of carbonation corrosion-resistant epoxy paint, it is characterised in that comprise the following steps：
(1) maleic anhydride of 2-3 parts by weight is taken, is added in the deionized water of 30-40 times of its weight, stirs, is added
The zinc acetylacetonate of 0.1-0.2 parts by weight, 60-70 DEG C is increased the temperature to, insulated and stirred 5-10 minutes, obtains acidification hydrolization liquid；
(2) pyrroles of 160-170 parts by weight is taken, is added in the tetrahydrofuran of 30-44 times of its weight, stirs, be sent to
In 60-70 DEG C of water bath with thermostatic control, the metallic potassium of 1-2 parts by weight is added, insulated and stirred 30-40 minutes, discharging cooling, adds 5-7
The paratoluensulfonyl chloride of parts by weight, magnetic agitation 20-24 hours, product is added in deionized water, stirred, stood
10-15 hours, filtering, sediment is washed, 1-2 hours are dried at 60-70 DEG C of vacuum, obtain sulphonylpyrroles；
(3) carbonic acid of 5-6 parts by weight is taken, is added in the deionized water of 20-30 times of its weight, stirs；
(4) above-mentioned acidification hydrolization liquid is taken, mixes, stirs with sulphonylpyrroles, ultrasonic 10-20 minutes, adds 0.3-1 weight
The alkanolamide, the silica of 13-15 parts by weight of part, stir, obtain acid amides pyrroles's dispersion liquid；
(5) phenol of 10-15 parts by weight is taken, heating melting, above-mentioned carbonate aqueous solution is added dropwise, insulated and stirred 10-20 minutes, adds
Sodium hydroxide, regulation pH are 7-8, stirring reaction 1-2 hours, obtain carbonization ester solution；
(6) above-mentioned acid amides pyrroles dispersion liquid, carbonization ester solution are mixed, stir, be sent in reactor, be passed through nitrogen,
It is 4-6 DEG C to adjust temperature of reaction kettle, insulation reaction 4-5 hours, is discharged, and filtering, sediment is washed, 70-75 DEG C of vacuum
Lower dry 20-23 hours, it is added in the deionized water of 100-110 times of its weight, ultrasonic 10-15 minutes, obtains silica and change
Property polypyrrole solution；
(7) epoxy resin of 130-140 parts by weight is taken, is mixed with above-mentioned silica modified polypyrrole solution, 4000-5000
Turn/part stirring 1-2 hours, obtain carbonation corrosion-resistant epoxy paint.
A kind of 2. preparation method of carbonation corrosion-resistant epoxy paint according to claim 1, it is characterised in that the carbon
The application method of Esterification corrosion-resistant epoxy paint is：Described carbonation corrosion-resistant epoxy paint is taken, with its weight 15-30%'s
Methylhexahydrophthalic anhydride mixes, and stirs, is coated to metallic substrate surface, the heat preservation solidification at 100-130 DEG C
100-150 minutes, you can.
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| CN201710392034.3A CN107177280B (en) | 2017-05-27 | 2017-05-27 | A kind of carbonation corrosion-resistant epoxy paint and preparation method thereof |
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| CN107177280B true CN107177280B (en) | 2018-04-06 |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105593321A (en) * | 2013-07-25 | 2016-05-18 | 日涂工业涂料有限公司 | Coating composition, coating film, and coated steel plate |
| CN106189815A (en) * | 2016-07-12 | 2016-12-07 | 天长市银狐漆业有限公司 | One is resistance to scrubs steel alloy anticorrosive paint and preparation method thereof |
| CN106189813A (en) * | 2016-07-12 | 2016-12-07 | 天长市银狐漆业有限公司 | A kind of Compound-acid modified alloy steel anticorrosive paint and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US9683109B2 (en) * | 2013-12-30 | 2017-06-20 | Council Of Scientific & Industrial Research | Self healing anti corrosive coatings and a process for the preparation thereof |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105593321A (en) * | 2013-07-25 | 2016-05-18 | 日涂工业涂料有限公司 | Coating composition, coating film, and coated steel plate |
| CN106189815A (en) * | 2016-07-12 | 2016-12-07 | 天长市银狐漆业有限公司 | One is resistance to scrubs steel alloy anticorrosive paint and preparation method thereof |
| CN106189813A (en) * | 2016-07-12 | 2016-12-07 | 天长市银狐漆业有限公司 | A kind of Compound-acid modified alloy steel anticorrosive paint and preparation method thereof |
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