CN104451626A - Galvanized steel sheet passivating agent and preparation method thereof - Google Patents
Galvanized steel sheet passivating agent and preparation method thereof Download PDFInfo
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- CN104451626A CN104451626A CN201410643235.2A CN201410643235A CN104451626A CN 104451626 A CN104451626 A CN 104451626A CN 201410643235 A CN201410643235 A CN 201410643235A CN 104451626 A CN104451626 A CN 104451626A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 229910001335 Galvanized steel Inorganic materials 0.000 title abstract 8
- 239000008397 galvanized steel Substances 0.000 title abstract 8
- 239000011347 resin Substances 0.000 claims abstract description 43
- 229920005989 resin Polymers 0.000 claims abstract description 43
- 239000000203 mixture Substances 0.000 claims abstract description 36
- 239000008367 deionised water Substances 0.000 claims abstract description 29
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 29
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 29
- 239000000945 filler Substances 0.000 claims abstract description 27
- IMQLKJBTEOYOSI-GPIVLXJGSA-N Inositol-hexakisphosphate Chemical compound OP(O)(=O)O[C@H]1[C@H](OP(O)(O)=O)[C@@H](OP(O)(O)=O)[C@H](OP(O)(O)=O)[C@H](OP(O)(O)=O)[C@@H]1OP(O)(O)=O IMQLKJBTEOYOSI-GPIVLXJGSA-N 0.000 claims abstract description 20
- IMQLKJBTEOYOSI-UHFFFAOYSA-N Phytic acid Natural products OP(O)(=O)OC1C(OP(O)(O)=O)C(OP(O)(O)=O)C(OP(O)(O)=O)C(OP(O)(O)=O)C1OP(O)(O)=O IMQLKJBTEOYOSI-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000004372 Polyvinyl alcohol Substances 0.000 claims abstract description 20
- 229940068041 phytic acid Drugs 0.000 claims abstract description 20
- 235000002949 phytic acid Nutrition 0.000 claims abstract description 20
- 239000000467 phytic acid Substances 0.000 claims abstract description 20
- 229920002451 polyvinyl alcohol Polymers 0.000 claims abstract description 20
- HLBBKKJFGFRGMU-UHFFFAOYSA-M sodium formate Chemical compound [Na+].[O-]C=O HLBBKKJFGFRGMU-UHFFFAOYSA-M 0.000 claims abstract description 20
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims abstract description 20
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims abstract description 19
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims abstract description 19
- RGPUVZXXZFNFBF-UHFFFAOYSA-K diphosphonooxyalumanyl dihydrogen phosphate Chemical compound [Al+3].OP(O)([O-])=O.OP(O)([O-])=O.OP(O)([O-])=O RGPUVZXXZFNFBF-UHFFFAOYSA-K 0.000 claims abstract description 19
- WXMKPNITSTVMEF-UHFFFAOYSA-M sodium benzoate Chemical compound [Na+].[O-]C(=O)C1=CC=CC=C1 WXMKPNITSTVMEF-UHFFFAOYSA-M 0.000 claims abstract description 19
- 235000010234 sodium benzoate Nutrition 0.000 claims abstract description 19
- 239000004299 sodium benzoate Substances 0.000 claims abstract description 19
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229910000831 Steel Inorganic materials 0.000 claims description 45
- 239000010959 steel Substances 0.000 claims description 45
- 238000003756 stirring Methods 0.000 claims description 24
- DZSVIVLGBJKQAP-UHFFFAOYSA-N 1-(2-methyl-5-propan-2-ylcyclohex-2-en-1-yl)propan-1-one Chemical compound CCC(=O)C1CC(C(C)C)CC=C1C DZSVIVLGBJKQAP-UHFFFAOYSA-N 0.000 claims description 19
- FSJSYDFBTIVUFD-SUKNRPLKSA-N (z)-4-hydroxypent-3-en-2-one;oxovanadium Chemical compound [V]=O.C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O FSJSYDFBTIVUFD-SUKNRPLKSA-N 0.000 claims description 18
- YCPXWRQRBFJBPZ-UHFFFAOYSA-N 5-sulfosalicylic acid Chemical compound OC(=O)C1=CC(S(O)(=O)=O)=CC=C1O YCPXWRQRBFJBPZ-UHFFFAOYSA-N 0.000 claims description 18
- 229940120146 EDTMP Drugs 0.000 claims description 18
- XQRLCLUYWUNEEH-UHFFFAOYSA-L diphosphonate(2-) Chemical compound [O-]P(=O)OP([O-])=O XQRLCLUYWUNEEH-UHFFFAOYSA-L 0.000 claims description 18
- NFDRPXJGHKJRLJ-UHFFFAOYSA-N edtmp Chemical compound OP(O)(=O)CN(CP(O)(O)=O)CCN(CP(O)(O)=O)CP(O)(O)=O NFDRPXJGHKJRLJ-UHFFFAOYSA-N 0.000 claims description 18
- 238000000034 method Methods 0.000 claims description 18
- -1 nitrilo trimethylene phosphonic acids Chemical class 0.000 claims description 18
- 235000019353 potassium silicate Nutrition 0.000 claims description 18
- 229960004418 trolamine Drugs 0.000 claims description 18
- 230000008569 process Effects 0.000 claims description 17
- 239000002994 raw material Substances 0.000 claims description 10
- 239000012467 final product Substances 0.000 claims description 8
- 239000000843 powder Substances 0.000 claims description 6
- 239000000377 silicon dioxide Substances 0.000 claims description 6
- 150000002118 epoxides Chemical class 0.000 claims description 4
- 239000005543 nano-size silicon particle Substances 0.000 claims description 4
- 235000012239 silicon dioxide Nutrition 0.000 claims description 4
- VAJVDSVGBWFCLW-UHFFFAOYSA-N 3-Phenyl-1-propanol Chemical compound OCCCC1=CC=CC=C1 VAJVDSVGBWFCLW-UHFFFAOYSA-N 0.000 claims description 3
- DYUQAZSOFZSPHD-UHFFFAOYSA-N Phenylpropyl alcohol Natural products CCC(O)C1=CC=CC=C1 DYUQAZSOFZSPHD-UHFFFAOYSA-N 0.000 claims description 3
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 3
- 229920000728 polyester Polymers 0.000 claims description 3
- 238000009413 insulation Methods 0.000 claims description 2
- 238000005260 corrosion Methods 0.000 abstract description 19
- 230000007797 corrosion Effects 0.000 abstract description 18
- 239000011651 chromium Substances 0.000 abstract description 6
- 229910052804 chromium Inorganic materials 0.000 abstract description 4
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 abstract description 3
- 238000007254 oxidation reaction Methods 0.000 abstract description 3
- 239000003795 chemical substances by application Substances 0.000 abstract 6
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 abstract 4
- LHTVOEBXFDDSQE-UHFFFAOYSA-N (1-hydroxy-1-phosphonooxyethyl) dihydrogen phosphate Chemical compound OP(=O)(O)OC(O)(C)OP(O)(O)=O LHTVOEBXFDDSQE-UHFFFAOYSA-N 0.000 abstract 2
- JKTORXLUQLQJCM-UHFFFAOYSA-N 4-phosphonobutylphosphonic acid Chemical compound OP(O)(=O)CCCCP(O)(O)=O JKTORXLUQLQJCM-UHFFFAOYSA-N 0.000 abstract 2
- 239000004115 Sodium Silicate Substances 0.000 abstract 2
- 239000004280 Sodium formate Substances 0.000 abstract 2
- YDONNITUKPKTIG-UHFFFAOYSA-N [Nitrilotris(methylene)]trisphosphonic acid Chemical compound OP(O)(=O)CN(CP(O)(O)=O)CP(O)(O)=O YDONNITUKPKTIG-UHFFFAOYSA-N 0.000 abstract 2
- 235000019254 sodium formate Nutrition 0.000 abstract 2
- 229910052911 sodium silicate Inorganic materials 0.000 abstract 2
- POILWHVDKZOXJZ-ARJAWSKDSA-M (z)-4-oxopent-2-en-2-olate Chemical compound C\C([O-])=C\C(C)=O POILWHVDKZOXJZ-ARJAWSKDSA-M 0.000 abstract 1
- 229920000536 2-Acrylamido-2-methylpropane sulfonic acid Polymers 0.000 abstract 1
- XHZPRMZZQOIPDS-UHFFFAOYSA-N 2-Methyl-2-[(1-oxo-2-propenyl)amino]-1-propanesulfonic acid Chemical compound OS(=O)(=O)CC(C)(C)NC(=O)C=C XHZPRMZZQOIPDS-UHFFFAOYSA-N 0.000 abstract 1
- WXHLLJAMBQLULT-UHFFFAOYSA-N 2-[[6-[4-(2-hydroxyethyl)piperazin-1-yl]-2-methylpyrimidin-4-yl]amino]-n-(2-methyl-6-sulfanylphenyl)-1,3-thiazole-5-carboxamide;hydrate Chemical compound O.C=1C(N2CCN(CCO)CC2)=NC(C)=NC=1NC(S1)=NC=C1C(=O)NC1=C(C)C=CC=C1S WXHLLJAMBQLULT-UHFFFAOYSA-N 0.000 abstract 1
- 229940088644 n,n-dimethylacrylamide Drugs 0.000 abstract 1
- YLGYACDQVQQZSW-UHFFFAOYSA-N n,n-dimethylprop-2-enamide Chemical compound CN(C)C(=O)C=C YLGYACDQVQQZSW-UHFFFAOYSA-N 0.000 abstract 1
- 235000019422 polyvinyl alcohol Nutrition 0.000 abstract 1
- 229910052814 silicon oxide Inorganic materials 0.000 abstract 1
- 235000019794 sodium silicate Nutrition 0.000 abstract 1
- 238000002161 passivation Methods 0.000 description 9
- 238000005246 galvanizing Methods 0.000 description 7
- 230000006872 improvement Effects 0.000 description 6
- 239000002245 particle Substances 0.000 description 6
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 238000012797 qualification Methods 0.000 description 4
- 239000003814 drug Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000000576 coating method Methods 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 241001163841 Albugo ipomoeae-panduratae Species 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 239000010960 cold rolled steel Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000009849 deactivation Effects 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000001934 delay Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000383 hazardous chemical Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 230000003449 preventive effect Effects 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 230000002269 spontaneous effect Effects 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 150000003585 thioureas Chemical class 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
- C23C22/06—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6
- C23C22/07—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing phosphates
Landscapes
- Chemical & Material Sciences (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Chemical Treatment Of Metals (AREA)
Abstract
The invention provides a galvanized steel sheet passivating agent and a preparation method thereof. The galvanized steel sheet passivating agent is prepared from the following components: phytic acid, 1-hydroxyl ethylidene bisphosphoric acid, nitrilotrimethylene phosphonic acid, ethanediamine tetramethylene phosphonic acid, sodium silicate, sodium formate, polyvinyl alcohol, sodium benzoate, triethanolamine, aluminum dihydrogen phosphate, sulfosalicylic acid, vanadiumoxy acetylacetonate, gamma-aminopropyltriethoxysilane, 2-acrylamido-2-methyl propane sulfonic acid, N, N-dimethyl acrylamide, silicon oxide filler, water-soluble film-forming resin and deionized water. The preparation method of the galvanized steel sheet passivating agent comprises the following steps: adding phytic acid, 1-hydroxyl ethylidene bisphosphoric acid, nitrilotrimethylene phosphonic acid, ethanediamine tetramethylene phosphonic acid, sodium silicate, sodium formate and polyvinyl alcohol into the deionized water, thereby forming a mixture I; then, mixing parts of the components with the deionized water, thereby forming a mixture II; and finally, mixing the mixture I with the mixture II, and then adding the residual components, thereby forming the galvanized steel sheet passivating agent. The galvanized steel sheet passivating agent does not contain chromium; and a galvanized steel sheet passivated by the galvanized steel sheet passivating agent has relatively high corrosion resistance and oxidization resistance.
Description
Technical field
The invention belongs to metal surface treatment chemical field, be specifically related to a kind of steel plate galvanized passivator and preparation method thereof.
Background technology
Metal passivation process instigates metallic surface due to the effect of medium, and be converted into not easily oxidized state, makes the method that corrosion of metal speed delays.The passivation of metal also may be spontaneous process (as generated the insoluble compound of one deck at metallic surface, i.e. oxide film).Be industrially, with passivator (mainly oxygenant), Passivation Treatment is carried out to metal, form layer protecting film.
Steel plate galvanized is one of important preventive means of cold-rolled steel sheet, and it is widely used in the industries such as aviation, electric power, traffic, building, machinery.Zincincation is mainly divided into electro-galvanizing and pot galvanize, wherein especially relatively simple with the manufacturing process of hot-dip galvanizing sheet steel, easily produces, therefore hot-dip galvanizing sheet steel in industry and daily application also widely.Hot-dip galvanizing sheet steel is used for the history of anticorrosion existing more than 200 year, still occupies an important position so far.In recent years, along with developing rapidly of construction industry, car industry and household electrical appliances industry, steel plate galvanized obtains to be applied more widely, also has higher requirement to the solidity to corrosion of hot-dip galvanizing sheet steel simultaneously.Steel plate galvanized easily corrodes, and makes Several Thiourea Derivatives on Zinc Plate Surface easily form ash dark-coloured, forms white rust or black change, generally need to carry out Passivation Treatment to improve corrosion resisting property in storage process.
Although steel plate galvanized has had stronger anti-corrosion capability, steel plate galvanized has still easily corroded in a humid environment, forms the corrosion product of white or becomes ash dead color, have impact on visual appearance and the coating corrosion stability of steel plate galvanized on its surface.Therefore, must process in the back segment operation of zincincation, improve the solidity to corrosion of steel plate, general aftertreatment comprises: phosphatization, passivation or organic coating process.Traditional hot-dip galvanizing sheet steel, general employing passivation aftertreatment improves its corrosion resistance nature, its common medicament all contains a large amount of sexavalent chromes, and from September, 2000, the European Parliament of ELV and cabinet member board of management instruction (EU instruction) specify Pd, Hg, Cd, Cr of auto production line
6+usage quantity limited, and enforcement: WEEE (waste electrical and electronicequipment) and RoHS (restriction of hazardous substances) instruction will be received in January, 2003 Bian about the EU instruction of electric appliance and electronic product, require that the household appliances after in July, 2006 use substitute materials to replace Cr
6+.Therefore, the Passivation Treatment being used in the hot-dip galvanizing sheet steel on automobile and household appliances cannot re-use containing Cr
6+medicament, or usage quantity will be limited, and this just needs exploitation chromium-free deactivation medicament to meet the needs in market and production.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art and provide a kind of steel plate galvanized passivator and preparation method thereof, this passivator is not containing chromium, environmentally friendly, and have higher corrosion resistance nature and oxidation resistent susceptibility by the steel plate galvanized of its passivation.
A kind of steel plate galvanized passivator, raw material comprises with parts by weight: phytic acid 4 ~ 12 parts, 1 hydroxyethylidine diphosphonate 3 ~ 10 parts, nitrilo trimethylene phosphonic acids 2 ~ 9 parts, ethylenediamine tetramethylene phosphonic acid 1 ~ 8 part, water glass 3 ~ 10 parts, sodium formiate 4 ~ 10 parts, polyvinyl alcohol 2 ~ 10 parts, Sodium Benzoate 1 ~ 9 part, trolamine 2 ~ 10 parts, aluminium dihydrogen phosphate 3 ~ 10 parts, sulphosalicylic acid 3 ~ 9 parts, vanadyl acetylacetonate 2 ~ 8 parts, γ-aminopropyl triethoxysilane 1 ~ 7 part, 2-acrylamide-2-methylpro panesulfonic acid 2 ~ 9 parts, N, N-DMAA 3 ~ 10 parts, cilicon oxide filler 0.8 ~ 4.2 part, water-soluble film-forming resin 5 ~ 18 parts, deionized water 10 ~ 25 parts.
As the further improvement of foregoing invention, described steel plate galvanized passivator, raw material comprises with parts by weight: phytic acid 6 ~ 10 parts, 1 hydroxyethylidine diphosphonate 4 ~ 9 parts, nitrilo trimethylene phosphonic acids 3 ~ 7 parts, ethylenediamine tetramethylene phosphonic acid 2 ~ 6 parts, water glass 4 ~ 9 parts, sodium formiate 6 ~ 9 parts, polyvinyl alcohol 4 ~ 9 parts, Sodium Benzoate 3 ~ 7 parts, trolamine 4 ~ 8 parts, aluminium dihydrogen phosphate 5 ~ 8 parts, sulphosalicylic acid 4 ~ 7 parts, vanadyl acetylacetonate 3 ~ 6 parts, γ-aminopropyl triethoxysilane 2 ~ 6 parts, 2-acrylamide-2-methylpro panesulfonic acid 4 ~ 8 parts, N, N-DMAA 5 ~ 9 parts, cilicon oxide filler 1.5 ~ 3.8 parts, water-soluble film-forming resin 7 ~ 16 parts, deionized water 14 ~ 22 parts.
As the further improvement of foregoing invention, described cilicon oxide filler is nano-silica powder or nano silicon dioxide sol.
As the further improvement of foregoing invention, described water-soluble film-forming resin is the one in water-soluble polyester film-forming resin, water-soluble phenylpropyl alcohol film-forming resin, soluble epoxide film-forming resin, aqurous ployurethane film-forming resin or water-soluble acrylic film-forming resin.
The preparation method of above-mentioned steel plate galvanized passivator, comprises the following steps:
Step 1, is added to phytic acid, 1 hydroxyethylidine diphosphonate, nitrilo trimethylene phosphonic acids, ethylenediamine tetramethylene phosphonic acid, water glass, sodium formiate and polyvinyl alcohol in 2/3 parts by weight of deionized water, stirs, obtain mixture I;
Step 2, mixes Sodium Benzoate, trolamine, aluminium dihydrogen phosphate, sulphosalicylic acid, vanadyl acetylacetonate, γ-aminopropyl triethoxysilane and residuals weight part deionized water, stirs, obtain mixture II;
Step 3, step 1 gained mixture I and step 2 gained mixture II are mixed, add 2-acrylamide-2-methylpro panesulfonic acid, N again, N-DMAA, cilicon oxide filler and water-soluble film-forming resin, stir, be heated to 40 ~ 60 DEG C, insulation 2 ~ 4h, be cooled to room temperature, obtain final product.
As the further improvement of foregoing invention, in step 1, the temperature of whipping process is 20 ~ 30 DEG C.
As the further improvement of foregoing invention, in step 2, the rotating speed of whipping process is 300 ~ 400rpm.
As the further improvement of foregoing invention, in step 3, insulating process carries out under vacuum tightness is 0.08 ~ 0.1MPa condition.
Passivator of the present invention is not containing chromium, environmentally friendly, and have higher corrosion resistance nature and oxidation resistent susceptibility by the steel plate galvanized of its passivation.
Embodiment
Embodiment 1
A kind of steel plate galvanized passivator, raw material comprises with parts by weight: phytic acid 4 parts, 1 hydroxyethylidine diphosphonate 3 parts, nitrilo trimethylene phosphonic acids 2 parts, ethylenediamine tetramethylene phosphonic acid 1 part, water glass 3 parts, sodium formiate 4 parts, polyvinyl alcohol 2 parts, Sodium Benzoate 1 part, trolamine 2 parts, aluminium dihydrogen phosphate 3 parts, sulphosalicylic acid 3 parts, vanadyl acetylacetonate 2 parts, γ-aminopropyl triethoxysilane 1 part, 2-acrylamide-2-methylpro panesulfonic acid 2 parts, N, N-DMAA 3 parts, cilicon oxide filler 0.8 part, water-soluble film-forming resin 5 parts, deionized water 10 parts.
Above-mentioned cilicon oxide filler is nano-silica powder, and particle diameter is 5 ~ 30nm; Water-soluble film-forming resin is water-soluble polyester film-forming resin.
The preparation method of above-mentioned steel plate galvanized passivator, comprises the following steps:
Step 1, is added in 2/3 parts by weight of deionized water by phytic acid, 1 hydroxyethylidine diphosphonate, nitrilo trimethylene phosphonic acids, ethylenediamine tetramethylene phosphonic acid, water glass, sodium formiate and polyvinyl alcohol, stirs, obtain mixture I under 20 DEG C of conditions;
Step 2, Sodium Benzoate, trolamine, aluminium dihydrogen phosphate, sulphosalicylic acid, vanadyl acetylacetonate, γ-aminopropyl triethoxysilane and residuals weight part deionized water are mixed, stir, the rotating speed of whipping process is 300rpm, obtains mixture II;
Step 3, step 1 gained mixture I and step 2 gained mixture II are mixed, add 2-acrylamide-2-methylpro panesulfonic acid, N again, N-DMAA, cilicon oxide filler and water-soluble film-forming resin, stir, be heated to 40 DEG C, vacuum tightness is be incubated 4h under 0.08MPa condition, be cooled to room temperature, obtain final product.
Embodiment 2
A kind of steel plate galvanized passivator, raw material comprises with parts by weight: phytic acid 6 parts, 1 hydroxyethylidine diphosphonate 4 parts, nitrilo trimethylene phosphonic acids 3 parts, ethylenediamine tetramethylene phosphonic acid 2 parts, water glass 4 parts, sodium formiate 6 parts, polyvinyl alcohol 4 parts, Sodium Benzoate 3 parts, trolamine 4 parts, aluminium dihydrogen phosphate 5 parts, sulphosalicylic acid 4 parts, vanadyl acetylacetonate 3 parts, γ-aminopropyl triethoxysilane 2 parts, 2-acrylamide-2-methylpro panesulfonic acid 4 parts, N, N-DMAA 5 parts, cilicon oxide filler 1.5 parts, water-soluble film-forming resin 7 parts, deionized water 14 parts.
Above-mentioned cilicon oxide filler is nano silicon dioxide sol, and particle diameter is 5 ~ 30nm; Water-soluble film-forming resin is water-soluble phenylpropyl alcohol film-forming resin.
The preparation method of above-mentioned steel plate galvanized passivator, comprises the following steps:
Step 1, is added in 2/3 parts by weight of deionized water by phytic acid, 1 hydroxyethylidine diphosphonate, nitrilo trimethylene phosphonic acids, ethylenediamine tetramethylene phosphonic acid, water glass, sodium formiate and polyvinyl alcohol, stirs, obtain mixture I under 25 DEG C of conditions;
Step 2, Sodium Benzoate, trolamine, aluminium dihydrogen phosphate, sulphosalicylic acid, vanadyl acetylacetonate, γ-aminopropyl triethoxysilane and residuals weight part deionized water are mixed, stir, the rotating speed of whipping process is 350rpm, obtains mixture II;
Step 3, step 1 gained mixture I and step 2 gained mixture II are mixed, add 2-acrylamide-2-methylpro panesulfonic acid, N again, N-DMAA, cilicon oxide filler and water-soluble film-forming resin, stir, be heated to 50 DEG C, vacuum tightness is be incubated 3h under 0.09MPa condition, be cooled to room temperature, obtain final product.
Embodiment 3
A kind of steel plate galvanized passivator, raw material comprises with parts by weight: phytic acid 9 parts, 1 hydroxyethylidine diphosphonate 5 parts, nitrilo trimethylene phosphonic acids 6 parts, ethylenediamine tetramethylene phosphonic acid 3 parts, water glass 5 parts, sodium formiate 8 parts, polyvinyl alcohol 7 parts, Sodium Benzoate 6 parts, trolamine 5 parts, aluminium dihydrogen phosphate 7 parts, sulphosalicylic acid 6 parts, vanadyl acetylacetonate 5 parts, γ-aminopropyl triethoxysilane 3 parts, 2-acrylamide-2-methylpro panesulfonic acid 7 parts, N, N-DMAA 7 parts, cilicon oxide filler 2.7 parts, water-soluble film-forming resin 12 parts, deionized water 19 parts.
Above-mentioned cilicon oxide filler is nano-silica powder, and particle diameter is 5 ~ 30nm; Water-soluble film-forming resin is soluble epoxide film-forming resin.
The preparation method of above-mentioned steel plate galvanized passivator, comprises the following steps:
Step 1, is added in 2/3 parts by weight of deionized water by phytic acid, 1 hydroxyethylidine diphosphonate, nitrilo trimethylene phosphonic acids, ethylenediamine tetramethylene phosphonic acid, water glass, sodium formiate and polyvinyl alcohol, stirs, obtain mixture I under 25 DEG C of conditions;
Step 2, Sodium Benzoate, trolamine, aluminium dihydrogen phosphate, sulphosalicylic acid, vanadyl acetylacetonate, γ-aminopropyl triethoxysilane and residuals weight part deionized water are mixed, stir, the rotating speed of whipping process is 400rpm, obtains mixture II;
Step 3, step 1 gained mixture I and step 2 gained mixture II are mixed, add 2-acrylamide-2-methylpro panesulfonic acid, N again, N-DMAA, cilicon oxide filler and water-soluble film-forming resin, stir, be heated to 45 DEG C, vacuum tightness is be incubated 4h under 0.08MPa condition, be cooled to room temperature, obtain final product.
Embodiment 4
A kind of steel plate galvanized passivator, raw material comprises with parts by weight: phytic acid 10 parts, 1 hydroxyethylidine diphosphonate 9 parts, nitrilo trimethylene phosphonic acids 7 parts, ethylenediamine tetramethylene phosphonic acid 6 parts, water glass 9 parts, sodium formiate 9 parts, polyvinyl alcohol 9 parts, Sodium Benzoate 7 parts, trolamine 8 parts, aluminium dihydrogen phosphate 8 parts, sulphosalicylic acid 7 parts, vanadyl acetylacetonate 6 parts, γ-aminopropyl triethoxysilane 6 parts, 2-acrylamide-2-methylpro panesulfonic acid 8 parts, N, N-DMAA 9 parts, cilicon oxide filler 3.8 parts, water-soluble film-forming resin 16 parts, deionized water 22 parts.
Above-mentioned cilicon oxide filler is nano-silica powder, and particle diameter is 5 ~ 30nm; Water-soluble film-forming resin is water-soluble acrylic film-forming resin.
The preparation method of above-mentioned steel plate galvanized passivator, comprises the following steps:
Step 1, is added in 2/3 parts by weight of deionized water by phytic acid, 1 hydroxyethylidine diphosphonate, nitrilo trimethylene phosphonic acids, ethylenediamine tetramethylene phosphonic acid, water glass, sodium formiate and polyvinyl alcohol, stirs, obtain mixture I under 30 DEG C of conditions;
Step 2, Sodium Benzoate, trolamine, aluminium dihydrogen phosphate, sulphosalicylic acid, vanadyl acetylacetonate, γ-aminopropyl triethoxysilane and residuals weight part deionized water are mixed, stir, the rotating speed of whipping process is 350rpm, obtains mixture II;
Step 3, step 1 gained mixture I and step 2 gained mixture II are mixed, add 2-acrylamide-2-methylpro panesulfonic acid, N again, N-DMAA, cilicon oxide filler and water-soluble film-forming resin, stir, be heated to 55 DEG C, vacuum tightness is be incubated 3h under 0.09MPa condition, be cooled to room temperature, obtain final product.
Embodiment 5
A kind of steel plate galvanized passivator, raw material comprises with parts by weight: phytic acid 12 parts, 1 hydroxyethylidine diphosphonate 10 parts, nitrilo trimethylene phosphonic acids 9 parts, ethylenediamine tetramethylene phosphonic acid 8 parts, water glass 10 parts, sodium formiate 10 parts, polyvinyl alcohol 10 parts, Sodium Benzoate 9 parts, trolamine 10 parts, aluminium dihydrogen phosphate 10 parts, sulphosalicylic acid 9 parts, vanadyl acetylacetonate 8 parts, γ-aminopropyl triethoxysilane 7 parts, 2-acrylamide-2-methylpro panesulfonic acid 9 parts, N, N-DMAA 10 parts, cilicon oxide filler 4.2 parts, water-soluble film-forming resin 18 parts, deionized water 25 parts.
Above-mentioned cilicon oxide filler is nano silicon dioxide sol, and particle diameter is 5 ~ 30nm; Water-soluble film-forming resin is aqurous ployurethane film-forming resin.
The preparation method of above-mentioned steel plate galvanized passivator, comprises the following steps:
Step 1, is added in 2/3 parts by weight of deionized water by phytic acid, 1 hydroxyethylidine diphosphonate, nitrilo trimethylene phosphonic acids, ethylenediamine tetramethylene phosphonic acid, water glass, sodium formiate and polyvinyl alcohol, stirs, obtain mixture I under 30 DEG C of conditions;
Step 2, Sodium Benzoate, trolamine, aluminium dihydrogen phosphate, sulphosalicylic acid, vanadyl acetylacetonate, γ-aminopropyl triethoxysilane and residuals weight part deionized water are mixed, stir, the rotating speed of whipping process is 400rpm, obtains mixture II;
Step 3, step 1 gained mixture I and step 2 gained mixture II are mixed, add 2-acrylamide-2-methylpro panesulfonic acid, N again, N-DMAA, cilicon oxide filler and water-soluble film-forming resin, stir, be heated to 60 DEG C, vacuum tightness is be incubated 2h under 0.06MPa condition, be cooled to room temperature, obtain final product.
Comparative example 1
The difference of the present embodiment and embodiment 3 is not comprise 2-acrylamide-2-methylpro panesulfonic acid in described passivator, specific as follows:
A kind of steel plate galvanized passivator, raw material comprises with parts by weight: phytic acid 9 parts, 1 hydroxyethylidine diphosphonate 5 parts, nitrilo trimethylene phosphonic acids 6 parts, ethylenediamine tetramethylene phosphonic acid 3 parts, water glass 5 parts, sodium formiate 8 parts, polyvinyl alcohol 7 parts, Sodium Benzoate 6 parts, trolamine 5 parts, aluminium dihydrogen phosphate 7 parts, sulphosalicylic acid 6 parts, vanadyl acetylacetonate 5 parts, γ-aminopropyl triethoxysilane 3 parts, N,N-DMAA 7 parts, cilicon oxide filler 2.7 parts, water-soluble film-forming resin 12 parts, deionized water 19 parts.
Above-mentioned cilicon oxide filler is nano-silica powder, and particle diameter is 5 ~ 30nm; Water-soluble film-forming resin is soluble epoxide film-forming resin.
The preparation method of above-mentioned steel plate galvanized passivator, comprises the following steps:
Step 1, is added in 2/3 parts by weight of deionized water by phytic acid, 1 hydroxyethylidine diphosphonate, nitrilo trimethylene phosphonic acids, ethylenediamine tetramethylene phosphonic acid, water glass, sodium formiate and polyvinyl alcohol, stirs, obtain mixture I under 25 DEG C of conditions;
Step 2, Sodium Benzoate, trolamine, aluminium dihydrogen phosphate, sulphosalicylic acid, vanadyl acetylacetonate, γ-aminopropyl triethoxysilane and residuals weight part deionized water are mixed, stir, the rotating speed of whipping process is 400rpm, obtains mixture II;
Step 3, mixes step 1 gained mixture I and step 2 gained mixture II, then adds N, N-DMAA, cilicon oxide filler and water-soluble film-forming resin, stir, and is heated to 45 DEG C, vacuum tightness is be incubated 4h under 0.08MPa condition, is cooled to room temperature, obtains final product.
By embodiment 1 to 5 gained passivator and comparative example 1 gained passivator, by the requirement specified in GB/T101251997, carry out neutral salt spray test, measure the corrosion resisting property of steel plate galvanized after 400 DEG C of baking 30s after passivator process respectively.It is qualified to be considered as by " salt-fog test 144h, corrosion area < 3% ".Result is as follows:
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Comparative example 1 | |
| Solidity to corrosion qualification rate (%) (1 day) | 99 | 98 | 100 | 97 | 97 | 70 |
| Solidity to corrosion qualification rate (%) (60 days) | 99 | 98 | 100 | 95 | 96 | 62 |
| Solidity to corrosion qualification rate (%) (120 days) | 99 | 96 | 100 | 94 | 96 | 56 |
| Solidity to corrosion qualification rate (%) (180 days) | 96 | 94 | 97 | 94 | 94 | 45 |
As seen from the above table, the protective film excellent corrosion resistance that formed of passivator of the present invention.Not comprising 2-acrylamide-2-methylpro panesulfonic acid in the passivator of comparative example 1 causes its solidity to corrosion obviously to decline; this may be because 2-acrylamide-2-methylpro panesulfonic acid can act synergistically with other components in passivator on the one hand, steel plate and extraneous corrosive medium are isolated; on the other hand when passive film is destroyed; can promote that effective constituent is oozed out; again passive film is generated with film surface action; make film have self-healing capability, still can have provide protection to steel plate galvanized.
Claims (8)
1. a steel plate galvanized passivator, it is characterized in that: raw material comprises with parts by weight: phytic acid 4 ~ 12 parts, 1 hydroxyethylidine diphosphonate 3 ~ 10 parts, nitrilo trimethylene phosphonic acids 2 ~ 9 parts, ethylenediamine tetramethylene phosphonic acid 1 ~ 8 part, water glass 3 ~ 10 parts, sodium formiate 4 ~ 10 parts, polyvinyl alcohol 2 ~ 10 parts, Sodium Benzoate 1 ~ 9 part, trolamine 2 ~ 10 parts, aluminium dihydrogen phosphate 3 ~ 10 parts, sulphosalicylic acid 3 ~ 9 parts, vanadyl acetylacetonate 2 ~ 8 parts, γ-aminopropyl triethoxysilane 1 ~ 7 part, 2-acrylamide-2-methylpro panesulfonic acid 2 ~ 9 parts, N, N-DMAA 3 ~ 10 parts, cilicon oxide filler 0.8 ~ 4.2 part, water-soluble film-forming resin 5 ~ 18 parts, deionized water 10 ~ 25 parts.
2. steel plate galvanized passivator according to claim 1, it is characterized in that: raw material comprises with parts by weight: phytic acid 6 ~ 10 parts, 1 hydroxyethylidine diphosphonate 4 ~ 9 parts, nitrilo trimethylene phosphonic acids 3 ~ 7 parts, ethylenediamine tetramethylene phosphonic acid 2 ~ 6 parts, water glass 4 ~ 9 parts, sodium formiate 6 ~ 9 parts, polyvinyl alcohol 4 ~ 9 parts, Sodium Benzoate 3 ~ 7 parts, trolamine 4 ~ 8 parts, aluminium dihydrogen phosphate 5 ~ 8 parts, sulphosalicylic acid 4 ~ 7 parts, vanadyl acetylacetonate 3 ~ 6 parts, γ-aminopropyl triethoxysilane 2 ~ 6 parts, 2-acrylamide-2-methylpro panesulfonic acid 4 ~ 8 parts, N, N-DMAA 5 ~ 9 parts, cilicon oxide filler 1.5 ~ 3.8 parts, water-soluble film-forming resin 7 ~ 16 parts, deionized water 14 ~ 22 parts.
3. steel plate galvanized passivator according to claim 1 and 2, is characterized in that: described cilicon oxide filler is nano-silica powder or nano silicon dioxide sol.
4. steel plate galvanized passivator according to claim 1 and 2, is characterized in that: described water-soluble film-forming resin is the one in water-soluble polyester film-forming resin, water-soluble phenylpropyl alcohol film-forming resin, soluble epoxide film-forming resin, aqurous ployurethane film-forming resin or water-soluble acrylic film-forming resin.
5. the preparation method of the steel plate galvanized passivator described in claim 1 or 2, is characterized in that: the preparation method of steel plate galvanized passivator, comprises the following steps:
Step 1, is added to phytic acid, 1 hydroxyethylidine diphosphonate, nitrilo trimethylene phosphonic acids, ethylenediamine tetramethylene phosphonic acid, water glass, sodium formiate and polyvinyl alcohol in 2/3 parts by weight of deionized water, stirs, obtain mixture I;
Step 2, mixes Sodium Benzoate, trolamine, aluminium dihydrogen phosphate, sulphosalicylic acid, vanadyl acetylacetonate, γ-aminopropyl triethoxysilane and residuals weight part deionized water, stirs, obtain mixture II;
Step 3, step 1 gained mixture I and step 2 gained mixture II are mixed, add 2-acrylamide-2-methylpro panesulfonic acid, N again, N-DMAA, cilicon oxide filler and water-soluble film-forming resin, stir, be heated to 40 ~ 60 DEG C, insulation 2 ~ 4h, be cooled to room temperature, obtain final product.
6. the preparation method of steel plate galvanized passivator according to claim 5, is characterized in that: in step 1, the temperature of whipping process is 20 ~ 30 DEG C.
7. the preparation method of steel plate galvanized passivator according to claim 5, is characterized in that: in step 2, the rotating speed of whipping process is 300 ~ 400rpm.
8. the preparation method of steel plate galvanized passivator according to claim 5, is characterized in that: in step 3, insulating process carries out under vacuum tightness is 0.08 ~ 0.1MPa condition.
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