CN108659676B - Preparation method of nitrite intercalation hydrotalcite material modified steel bar epoxy resin coating - Google Patents
Preparation method of nitrite intercalation hydrotalcite material modified steel bar epoxy resin coating Download PDFInfo
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- CN108659676B CN108659676B CN201810583740.0A CN201810583740A CN108659676B CN 108659676 B CN108659676 B CN 108659676B CN 201810583740 A CN201810583740 A CN 201810583740A CN 108659676 B CN108659676 B CN 108659676B
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- 239000003822 epoxy resin Substances 0.000 title claims abstract description 80
- 229920000647 polyepoxide Polymers 0.000 title claims abstract description 80
- GDVKFRBCXAPAQJ-UHFFFAOYSA-A dialuminum;hexamagnesium;carbonate;hexadecahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Al+3].[Al+3].[O-]C([O-])=O GDVKFRBCXAPAQJ-UHFFFAOYSA-A 0.000 title claims abstract description 67
- 229910001701 hydrotalcite Inorganic materials 0.000 title claims abstract description 66
- 229960001545 hydrotalcite Drugs 0.000 title claims abstract description 66
- 239000000463 material Substances 0.000 title claims abstract description 51
- 238000000576 coating method Methods 0.000 title claims abstract description 50
- IOVCWXUNBOPUCH-UHFFFAOYSA-M Nitrite anion Chemical compound [O-]N=O IOVCWXUNBOPUCH-UHFFFAOYSA-M 0.000 title claims abstract description 49
- 239000011248 coating agent Substances 0.000 title claims abstract description 45
- 238000009830 intercalation Methods 0.000 title claims abstract description 32
- 230000002687 intercalation Effects 0.000 title claims abstract description 32
- 229910000831 Steel Inorganic materials 0.000 title claims abstract description 22
- 239000010959 steel Substances 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000003960 organic solvent Substances 0.000 claims abstract description 31
- 239000011259 mixed solution Substances 0.000 claims abstract description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 27
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000000243 solution Substances 0.000 claims abstract description 26
- 239000006185 dispersion Substances 0.000 claims abstract description 24
- 239000000843 powder Substances 0.000 claims abstract description 24
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims abstract description 22
- 229910000077 silane Inorganic materials 0.000 claims abstract description 22
- 239000004952 Polyamide Substances 0.000 claims abstract description 18
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 18
- 229920002647 polyamide Polymers 0.000 claims abstract description 18
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims abstract description 17
- 238000001291 vacuum drying Methods 0.000 claims abstract description 16
- 239000008367 deionised water Substances 0.000 claims abstract description 14
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 14
- 230000007935 neutral effect Effects 0.000 claims abstract description 13
- 238000000926 separation method Methods 0.000 claims abstract description 11
- 238000005406 washing Methods 0.000 claims abstract description 11
- 238000001132 ultrasonic dispersion Methods 0.000 claims abstract description 10
- 238000000227 grinding Methods 0.000 claims abstract description 8
- 238000003760 magnetic stirring Methods 0.000 claims abstract description 7
- 239000000126 substance Substances 0.000 claims abstract description 6
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 18
- LPXPTNMVRIOKMN-UHFFFAOYSA-M sodium nitrite Chemical compound [Na+].[O-]N=O LPXPTNMVRIOKMN-UHFFFAOYSA-M 0.000 claims description 16
- 230000003647 oxidation Effects 0.000 claims description 12
- 238000007254 oxidation reaction Methods 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 10
- 235000010288 sodium nitrite Nutrition 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 7
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims description 6
- 239000012153 distilled water Substances 0.000 claims description 6
- 235000019441 ethanol Nutrition 0.000 claims description 6
- 235000006408 oxalic acid Nutrition 0.000 claims description 6
- 239000002994 raw material Substances 0.000 claims description 5
- 239000003054 catalyst Substances 0.000 claims description 2
- 230000007797 corrosion Effects 0.000 abstract description 27
- 238000005260 corrosion Methods 0.000 abstract description 27
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 abstract description 10
- 239000011148 porous material Substances 0.000 abstract description 6
- 230000009545 invasion Effects 0.000 abstract description 2
- 230000035515 penetration Effects 0.000 abstract description 2
- 230000007547 defect Effects 0.000 description 7
- 229920006334 epoxy coating Polymers 0.000 description 7
- 239000004593 Epoxy Substances 0.000 description 6
- 229910001294 Reinforcing steel Inorganic materials 0.000 description 6
- 239000004567 concrete Substances 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 238000000840 electrochemical analysis Methods 0.000 description 5
- 230000004048 modification Effects 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 229910001051 Magnalium Inorganic materials 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 239000000945 filler Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- -1 nitrite ions Chemical class 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 239000011256 inorganic filler Substances 0.000 description 2
- 229910003475 inorganic filler Inorganic materials 0.000 description 2
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 2
- 239000011150 reinforced concrete Substances 0.000 description 2
- 230000002787 reinforcement Effects 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 239000011800 void material Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 230000001939 inductive effect Effects 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
- 229910001845 yogo sapphire Inorganic materials 0.000 description 1
Classifications
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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
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Paints Or Removers (AREA)
- Epoxy Resins (AREA)
Abstract
The invention provides a preparation method of a nitrite intercalation hydrotalcite material modified steel bar epoxy resin coating material, which is characterized by comprising the following steps: adding nitrite intercalation hydrotalcite material and silane into a silane organic mixed solution according to a certain mass ratio, carrying out water bath magnetic stirring, carrying out separation treatment, washing with a mixed solution of ethanol and deionized water until the pH value is neutral, and carrying out vacuum drying to obtain a dried substance; grinding the dried substance into fine powder, adding the fine powder into an n-butanol organic solvent, and performing ultrasonic dispersion to obtain an organic solvent dispersion solution; adding epoxy resin into the organic solvent dispersion solution, and performing ultrasonic dispersion; adding a polyamide curing agent, uniformly dispersing, and performing vacuum drying to obtain the polyamide curing agent; the invention can not only compact the pore structure of the epoxy resin, block the penetration and invasion of chloride ions and prevent the occurrence of the corrosion of the chloride ions of the steel bar, thereby leading the coating material to have multifunctionality and intelligence and greatly improving the corrosion protection capability of the epoxy resin coating to the steel bar.
Description
Technical Field
The invention belongs to the technical field of reinforcement corrosion protection in concrete, and particularly relates to a nitrite intercalated hydrotalcite material modified reinforcement epoxy resin coating and a preparation method thereof.
Background
The reinforced bar chloride ion corrosion is the main reason for reducing the durability of the concrete structure and shortening the service life, which causes great damage to national economy and life safety of people, and the reinforced bar corrosion problem caused by chloride ion corrosion appears 5-10 years after many marine concrete structure projects in China are used.
Nevertheless, the epoxy resin coating often has some tiny void defects during the coating process, thereby inducing pitting corrosion, and once the pitting corrosion occurs, large cathodes and small anodes are generated, thereby accelerating the corrosion of the steel bars and drastically reducing the durability of the epoxy resin coated reinforced concrete structure, at present, modification treatment such as doping with nano Al2O3, graphene particles, nano ZnO and the like is often performed to improve the performance of the epoxy resin coating, but these inorganic fillers are single-functional and only compact the microstructure; meanwhile, there is a problem in that the coating adhesive property is lowered due to poor compatibility between the inorganic filler and the organic epoxy resin.
Disclosure of Invention
The purpose of the invention is as follows: in order to overcome the defects, the invention provides a reinforcing steel bar epoxy resin coating modified by nitrite intercalation hydrotalcite material and a preparation method thereof, the nano hydrotalcite material is easy to exchange interlayer anions due to a unique lamellar structure, can be often used as an adsorbent of chloride ions, and is a pillared hydrotalcite material assembled by taking nitrite as an object, and after the nano hydrotalcite material is organically modified, the pillared hydrotalcite material is used as a filler of epoxy resin, so that not only can the pore structure be compacted, but also the problem of compatibility can be solved due to good compatibility of the organically modified hydrotalcite and the epoxy resin. In addition, the nitrite intercalation hydrotalcite material can absorb chloride ions in the coating and release nitrite ions with rust resistance, so that the coating has the characteristics of multifunction and intelligence, and the corrosion protection capability of the epoxy resin coating on the steel bar is greatly improved.
Aiming at the defects of the prior art, the nitrite intercalation hydrotalcite material is used as a filler, the filler is organically modified and uniformly dispersed in epoxy resin, so that the nitrite intercalation hydrotalcite material modified steel bar epoxy resin coating is prepared.
A preparation method of a nitrite intercalated hydrotalcite material modified steel bar epoxy resin coating material comprises the following steps:
the method comprises the following steps: adding a nitrite intercalation hydrotalcite material into a silane organic mixed solution according to the mass ratio of 1: 1-2 of the nitrite intercalation hydrotalcite material to silane, carrying out water bath magnetic stirring at 60-80 ℃ for 3-6 hours, carrying out separation treatment, washing with a mixed solution of ethanol and deionized water until the pH value is neutral, and carrying out vacuum drying to obtain a dried substance;
step two: grinding the dried substance into fine powder, adding the fine powder into an n-butyl alcohol organic solvent, and ultrasonically dispersing for 0.5-1 h to prepare an organic solvent dispersion solution;
step three: adding epoxy resin into the organic solvent dispersion solution, and ultrasonically dispersing for 0.5-1 h at the constant temperature of 50-60 ℃;
wherein, the adding amount of the fine powder in the second step is 0.1 to 1.5 percent of the mass of the epoxy resin;
step four: adding polyamide curing agent, dispersing uniformly, and vacuum drying for 20-60 min to obtain the product.
Further, the preparation method of the nitrite intercalation hydrotalcite material comprises the following steps: carbonate hydrotalcite is used as a raw material, is roasted at the temperature of 450-550 ℃ to obtain a roasted oxidation product, is mixed with sodium nitrite, is added into distilled water which is boiled twice, is stirred for 3-6 h at the temperature of 85-100 ℃, is separated, is washed until the pH value is neutral, and is dried in vacuum, so that the catalyst is obtained.
Further, the molar ratio of the calcined oxidation product to sodium nitrite is 1: 2-5, mixing.
Further, the preparation method of the silane organic mixed solution comprises the following steps: preparing a mixed solution of absolute ethyl alcohol and deionized water according to the mass ratio of 1: 5-1: 15, adding silane with the mass concentration of 5% -30% into the mixed solution, adjusting the pH value to 4-5 by using oxalic acid, and performing ultrasonic dispersion for 10-30 min to obtain the product.
Furthermore, the addition amount of the epoxy resin in the third step is 5-10 times of the mass of the organic solvent dispersion solution, and the addition amount of the polyamide curing agent in the fourth step is 30-60% of the mass of the epoxy resin.
Furthermore, the adding amount of the fine powder in the second step is 0.1 percent of the mass of the epoxy resin, the adding amount of the epoxy resin in the third step is 5 times of the mass of the organic solvent dispersion solution, and the adding amount of the polyamide curing agent in the fourth step is 30 percent of the mass of the epoxy resin.
Furthermore, the adding amount of the fine powder in the second step is 0.3 percent of the mass of the epoxy resin, the adding amount of the epoxy resin in the third step is 7 times of the mass of the organic solvent dispersion solution, and the adding amount of the polyamide curing agent in the fourth step is 40 percent of the mass of the epoxy resin.
Furthermore, the adding amount of the fine powder in the second step is 0.5 percent of the mass of the epoxy resin, the adding amount of the epoxy resin in the third step is 8 times of the mass of the organic solvent dispersion solution, and the adding amount of the polyamide curing agent in the fourth step is 50 percent of the mass of the epoxy resin.
Furthermore, the adding amount of the fine powder in the second step is 1% of the mass of the epoxy resin, the adding amount of the epoxy resin in the third step is 10 times of the mass of the organic solvent dispersion solution, and the adding amount of the polyamide curing agent in the fourth step is 60% of the mass of the epoxy resin.
A nitrite intercalation hydrotalcite material modified steel bar epoxy resin coating material, which is prepared by the preparation method.
Has the advantages that: the nitrite intercalation hydrotalcite material is used as a modified material, and is organically modified, so that the compatibility of the nitrite intercalation hydrotalcite and the epoxy resin coating is effectively improved, and the bonding property of the reinforcing steel bar epoxy resin coating is improved; in addition, the pore structure of the epoxy resin can be compacted to block the penetration and invasion of chloride ions; meanwhile, the penetrated chloride ions can be effectively adsorbed and released to release corrosion inhibition ions nitrite, so that the corrosion of the chloride ions of the steel bar is prevented, the epoxy resin coating has multifunctionality and intelligence, and the corrosion protection capability of the epoxy resin coating on the steel bar is greatly improved; the preparation method is simple and efficient, the coating has great practical significance for improving the durability of the reinforced concrete structure in the chloride environment, and the coating is easy to popularize and industrialize and has wide application prospect.
The specific implementation mode is as follows:
the present invention is further illustrated by the following examples, which are intended to be purely exemplary and are not intended to limit the scope of the invention, as various equivalent modifications of the invention will occur to those skilled in the art upon reading the present disclosure and fall within the scope of the appended claims.
Firstly, selecting an HPB235 reinforcing steel bar, processing the reinforcing steel bar into a small cylinder with the thickness of 15mm multiplied by 4mm, removing oil and dirt, welding a copper wire on one end face of the reinforcing steel bar, fixedly sealing the end face and the cylinder face by using epoxy, gradually grinding and polishing the reinforcing steel bar without epoxy sealing to a mirror surface by using metallographic abrasive paper, cleaning by using acetone and deionized water, drying, and coating an epoxy layer on a coater, wherein the area of a working surface is 1.767cm2, namely the prepared modified epoxy resin coating surface, the thickness of the coating is controlled to be 60 +/-5 mu m, the coating is used as a working electrode for corrosion electrochemical test, and a corrosion medium during the test is a 3.5 percent NaCl solution prepared from a saturated Ca (OH) solution.
The first embodiment is as follows:
a, using carbonate hydrotalcite synthesized by a coprecipitation method as a raw material, roasting for 8 hours at 480 ℃ to obtain a roasted oxidation product, and mixing the roasted oxidation product with sodium nitrite according to a molar ratio of 1:2, mixing, adding into distilled water boiled twice, stirring for 3h at 80 ℃, performing centrifugal separation treatment, washing until the pH value is neutral, and performing vacuum drying to obtain the nitrite intercalation hydrotalcite material;
b, preparing a mixed solution of absolute ethyl alcohol and deionized water according to the mass ratio of 1:5, adding silane with the mass concentration of 10% into the mixed solution, adjusting the pH value to 4 by using oxalic acid, and performing ultrasonic dispersion for 30 min;
adding nitrite intercalated hydrotalcite and silane into the silane organic mixed solution according to the mass ratio of 1:1, carrying out water bath magnetic stirring at 60 ℃ for 3 hours, carrying out separation treatment, washing with a mixed solution of ethanol and deionized water until the pH value is neutral, and carrying out vacuum drying;
grinding the nitrite intercalation hydrotalcite to fine powder, adding the fine powder into an n-butanol organic solvent according to the mass concentration of 0.1% (relative to the mass of the epoxy resin), and ultrasonically dispersing for 0.5 h;
adding 5 times of epoxy resin (relative to the organic solvent dispersion solution) into the nitrite intercalation hydrotalcite organic solvent dispersion solution, and ultrasonically dispersing for 0.5h at the constant temperature of 50 ℃;
f, adding a polyamide curing agent accounting for 30 percent of the mass of the epoxy resin, uniformly dispersing, and drying in vacuum for 20min to remove bubbles.
The results of the electrochemical tests after the application of the epoxy coating show that: before being soaked in corrosive medium, the impedance value is 7.5 multiplied by 1010 omega cm23.9X 109. omega. cm for coatings less doped with hydrotalcite2The improvement of one order of magnitude shows that the compactness of the modified epoxy coating is greatly improved, the repairing effect on the microscopic pore defects of the epoxy is obvious, and the corrosion resistant period (the corrosion potential is reduced to be below-600 mV) of the modified epoxy coating is different from that of the coating without the hydrotalcite20d is increased to about 65 d.
The second embodiment is as follows:
a, roasting carbonate hydrotalcite prepared by a hydrothermal synthesis method at 500 ℃ for 6 hours to obtain a roasted oxidation product, mixing the oxidation product with sodium nitrite according to a molar ratio of 1:3, adding the mixture into distilled water boiled twice, stirring for 4 hours at 85 ℃, performing centrifugal separation treatment, washing until the pH value is neutral, and performing vacuum drying to obtain a nitrite intercalation hydrotalcite material;
b, preparing a mixed solution of absolute ethyl alcohol and deionized water according to the mass ratio of 1:8, adding silane with the mass concentration of 20% into the mixed solution, adjusting the pH value to 4 by using oxalic acid, and performing ultrasonic dispersion for 25 min;
adding nitrite intercalated hydrotalcite and silane into the silane organic mixed solution according to the mass ratio of 1:1.5, carrying out water bath magnetic stirring at 70 ℃ for 4 hours, carrying out separation treatment, washing with a mixed solution of ethanol and deionized water until the pH value is neutral, and carrying out vacuum drying;
grinding the nitrite intercalated hydrotalcite to fine powder, adding the fine powder into an n-butanol organic solvent according to the mass concentration of 0.3 percent (relative to the mass of the epoxy resin), and performing ultrasonic dispersion for 0.5 h;
e, adding 7 times of epoxy resin (relative to the organic solvent dispersion solution) into the nitrite intercalation hydrotalcite organic solvent dispersion solution, and ultrasonically dispersing for 0.6h at the constant temperature of 55 ℃;
f, adding a polyamide curing agent accounting for 40% of the mass of the epoxy resin, uniformly dispersing, and carrying out vacuum drying for 30min to remove bubbles.
The results of the electrochemical tests after the application of the epoxy coating show that: before the corrosion medium is soaked, the impedance value is 1.5 multiplied by 1010 omega cm23.9X 109. omega. cm for coatings less doped with hydrotalcite2The obvious improvement shows that the repairing effect on the micro-pore defects of the epoxy is obvious, and the corrosion resistant period (the corrosion potential is reduced to be below-600 mV) is improved from 20d of the coating without the hydrotalcite to about 50 d.
The third concrete implementation mode:
a, using commercial or synthetic carbonate hydrotalcite as a raw material, roasting for 4 hours at 520 ℃ to obtain a roasted oxidation product, mixing the oxidation product with sodium nitrite according to the molar ratio of 1:4, adding the mixture into distilled water which is boiled twice, stirring for 5 hours at 90 ℃, carrying out centrifugal separation treatment, washing until the pH value is neutral, and carrying out vacuum drying to obtain a nitrite intercalation hydrotalcite material;
b, preparing a mixed solution of absolute ethyl alcohol and deionized water according to the mass ratio of 1:10, adding silane with the mass concentration of 30% into the mixed solution, adjusting the pH value to 5 by using oxalic acid, and performing ultrasonic dispersion for 20 min;
adding nitrite intercalated hydrotalcite and silane into the silane organic mixed solution according to the mass ratio of 1:1.5, carrying out water bath magnetic stirring at 75 ℃ for 5 hours, carrying out separation treatment, washing with a mixed solution of ethanol and deionized water until the pH value is neutral, and carrying out vacuum drying;
grinding the nitrite intercalated hydrotalcite to fine powder, adding the fine powder into an n-butanol organic solvent according to the mass concentration of 0.5 percent (relative to the mass of the epoxy resin), and ultrasonically dispersing for 0.8 h;
adding 8 times of epoxy resin (relative to the organic solvent dispersion solution) into the nitrite intercalation hydrotalcite organic solvent dispersion solution, and ultrasonically dispersing for 0.8h at the constant temperature of 60 ℃;
and e, adding a polyamide curing agent accounting for 50% of the mass of the epoxy resin, uniformly dispersing, and carrying out vacuum drying for 40min to remove bubbles.
The results of the electrochemical tests after the application of the epoxy coating show that: before the corrosion medium is soaked, the impedance value is 7.5 multiplied by 109 omega cm23.9X 109. omega. cm for coatings less doped with hydrotalcite2The obvious improvement shows that the repairing effect on the micro-pore defects of the epoxy is obvious and the corrosion resistant period (the corrosion potential is reduced to be below-600 mV) is improved from 20d of the coating without the hydrotalcite to about 35 d.
The fourth concrete implementation mode:
a, using commercial or synthetic carbonate hydrotalcite as a raw material, roasting for 3 hours at 550 ℃ to obtain a roasted oxidation product, mixing the oxidation product with sodium nitrite according to the mass ratio of 1:4, adding the mixture into distilled water which is boiled twice, stirring for 6 hours at 95 ℃, carrying out centrifugal separation treatment, washing until the pH value is neutral, and carrying out vacuum drying to obtain a nitrite intercalation hydrotalcite material;
b, preparing a mixed solution of absolute ethyl alcohol and deionized water according to the mass ratio of 1:15, adding silane with the mass concentration of 5% into the mixed solution, adjusting the pH value to 5 by using oxalic acid, and performing ultrasonic dispersion for 10 min;
adding nitrite intercalated hydrotalcite and silane into the silane organic mixed solution according to the mass ratio of 1:2, carrying out water bath magnetic stirring at 80 ℃ for 6 hours, carrying out separation treatment, washing with a mixed solution of ethanol and deionized water until the pH value is neutral, and carrying out vacuum drying;
grinding the nitrite intercalated hydrotalcite to fine powder, adding the fine powder into an n-butyl alcohol organic solvent according to the mass concentration of 1% (relative to the mass of the epoxy resin), and performing ultrasonic dispersion for 1 hour;
e, adding 10 times of epoxy resin (relative to the organic solvent dispersion solution) into the nitrite intercalation hydrotalcite organic solvent dispersion solution, and ultrasonically dispersing for 1h at the constant temperature of 60 ℃;
f, adding a polyamide curing agent accounting for 60 percent of the mass of the epoxy resin, uniformly dispersing, and drying in vacuum for 60min to remove bubbles.
The results of the electrochemical tests after the application of the epoxy coating show that: before the corrosion medium is soaked, the impedance value is 4.5 multiplied by 1010 omega cm23.9X 109. omega. cm for coatings less doped with hydrotalcite2The corrosion resistance period (the corrosion potential is reduced to below-600 mV) of the coating without the hydrotalcite is improved to about 30 days from 20 days of the coating without the hydrotalcite, so the later-stage rust resistance effect of the doping amount is obvious.
According to the embodiment, under the same preparation process, 0.1-1.5% of the epoxy resin coating modified by the nitrite intercalation magnalium hydrotalcite is greatly improved in the aspects of the impedance and corrosion resistant period of the coating compared with the blank epoxy coating not modified by the nitrite intercalation magnalium hydrotalcite, and a microscopic scanning electron microscope shows that the porosity and void defects of the coating can be reduced by doping the nitrite intercalation magnalium hydrotalcite, so that the coating has a great improvement effect on the microstructure.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A preparation method of a nitrite intercalated hydrotalcite material modified steel bar epoxy resin coating material is characterized by comprising the following steps:
the method comprises the following steps: adding a nitrite intercalation hydrotalcite material into a silane organic mixed solution according to the mass ratio of 1: 1-2 of the nitrite intercalation hydrotalcite material to silane, carrying out water bath magnetic stirring at 60-80 ℃ for 3-6 hours, carrying out separation treatment, washing with a mixed solution of ethanol and deionized water until the pH value is neutral, and carrying out vacuum drying to obtain a dried substance;
step two: grinding the dried substance into fine powder, adding the fine powder into an n-butyl alcohol organic solvent, and ultrasonically dispersing for 0.5-1 h to prepare an organic solvent dispersion solution;
step three: adding epoxy resin into the organic solvent dispersion solution, and ultrasonically dispersing for 0.5-1 h at the constant temperature of 50-60 ℃;
wherein, the adding amount of the fine powder in the second step is 0.1 to 1.5 percent of the mass of the epoxy resin;
step four: adding polyamide curing agent, dispersing uniformly, and vacuum drying for 20-60 min to obtain the product.
2. The method for preparing the nitrite intercalation hydrotalcite material modified steel bar epoxy resin coating material according to the claim 1, wherein the nitrite intercalation hydrotalcite material is prepared by the following steps: carbonate hydrotalcite is used as a raw material, is roasted at the temperature of 450-550 ℃ to obtain a roasted oxidation product, is mixed with sodium nitrite, is added into distilled water which is boiled twice, is stirred for 3-6 h at the temperature of 85-100 ℃, is separated, is washed until the pH value is neutral, and is dried in vacuum, so that the catalyst is obtained.
3. The method for preparing the nitrite intercalation hydrotalcite material modified steel bar epoxy resin coating material as claimed in claim 2, wherein the molar ratio of the roasted oxidation product to the sodium nitrite is 1: 2-5, mixing.
4. The preparation method of the nitrite intercalated hydrotalcite material modified steel bar epoxy resin coating material as claimed in claim 1, wherein the preparation method of the silane organic mixed solution comprises the following steps: preparing a mixed solution of absolute ethyl alcohol and deionized water according to the mass ratio of 1: 5-1: 15, adding silane with the mass concentration of 5% -30% into the mixed solution, adjusting the pH value to 4-5 by using oxalic acid, and performing ultrasonic dispersion for 10-30 min to obtain the product.
5. The preparation method of the nitrite intercalated hydrotalcite material modified steel bar epoxy resin coating material as claimed in claim 1, wherein the addition amount of the epoxy resin in the third step is 5-10 times of the mass of the organic solvent dispersion solution, and the addition amount of the polyamide curing agent in the fourth step is 30-60% of the mass of the epoxy resin.
6. The method for preparing the nitrite intercalated hydrotalcite material modified steel bar epoxy resin coating material as claimed in claim 5, wherein the addition amount of the fine powder in the second step is 0.1% of the mass of the epoxy resin, the addition amount of the epoxy resin in the third step is 5 times of the mass of the organic solvent dispersion solution, and the addition amount of the polyamide curing agent in the fourth step is 30% of the mass of the epoxy resin.
7. The method for preparing the nitrite intercalated hydrotalcite material modified steel bar epoxy resin coating material as claimed in claim 5, wherein the addition amount of the fine powder in the second step is 0.3% of the mass of the epoxy resin, the addition amount of the epoxy resin in the third step is 7 times of the mass of the organic solvent dispersion solution, and the addition amount of the polyamide curing agent in the fourth step is 40% of the mass of the epoxy resin.
8. The method for preparing the nitrite intercalated hydrotalcite material modified steel bar epoxy resin coating material as claimed in claim 5, wherein the addition amount of the fine powder in the second step is 0.5% of the mass of the epoxy resin, the addition amount of the epoxy resin in the third step is 8 times of the mass of the organic solvent dispersion solution, and the addition amount of the polyamide curing agent in the fourth step is 50% of the mass of the epoxy resin.
9. The method for preparing the nitrite intercalated hydrotalcite material modified steel bar epoxy resin coating material as claimed in claim 5, wherein the addition amount of the fine powder in the second step is 1% of the mass of the epoxy resin, the addition amount of the epoxy resin in the third step is 10 times of the mass of the organic solvent dispersion solution, and the addition amount of the polyamide curing agent in the fourth step is 60% of the mass of the epoxy resin.
10. A nitrite intercalation hydrotalcite material modified steel bar epoxy resin coating material, which is characterized by being prepared by the preparation method of any one of claims 1 to 9.
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