CN106700701A - High temperature resistance environment-friendly Dacromet paint, preparation method thereof, high temperature resistance environment-friendly Dacromet coating and preparation method thereof - Google Patents
High temperature resistance environment-friendly Dacromet paint, preparation method thereof, high temperature resistance environment-friendly Dacromet coating and preparation method thereof Download PDFInfo
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- CN106700701A CN106700701A CN201611019186.0A CN201611019186A CN106700701A CN 106700701 A CN106700701 A CN 106700701A CN 201611019186 A CN201611019186 A CN 201611019186A CN 106700701 A CN106700701 A CN 106700701A
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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
- C09D5/10—Anti-corrosive paints containing metal dust
- C09D5/103—Anti-corrosive paints containing metal dust containing Al
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- 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
- C09D1/00—Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances
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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
- C09D5/10—Anti-corrosive paints containing metal dust
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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
- C09D5/10—Anti-corrosive paints containing metal dust
- C09D5/106—Anti-corrosive paints containing metal dust containing Zn
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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
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/63—Additives non-macromolecular organic
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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
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/65—Additives macromolecular
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- 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
- C23C22/40—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 molybdates, tungstates or vanadates
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- 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
- C23C2222/00—Aspects relating to chemical surface treatment of metallic material by reaction of the surface with a reactive medium
- C23C2222/20—Use of solutions containing silanes
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Abstract
The invention belongs to the field of material corrosion resistance, and particularly relates to a high temperature resistance environment-friendly Dacromet paint, a preparation method thereof, a high temperature resistance environment-friendly Dacromet coating and a preparation method thereof. The environment-friendly Dacromet paint comprises the following ingredients in parts by weight: 45-50% of metal slurry, 45-50% of chromate-free passivation liquid and 2-5% of relevant accessory ingredient, wherein the metal powder consists of flake zinc powder, flake aluminum powder, flake magnesium powder and flake manganese powder at the ratio of 4:1:1:1-8:1:1:1. According to the high temperature resistance environment-friendly Dacromet paint disclosed by the invention, the magnesium powder and the manganese powder are selected to replace parts of zinc powder, absolute ethyl alcohol is used for replacing water, and therefore, the problem that a traditional Dacromet coating loses efficacy due to the inversion of the electrode electric potential of the zinc powder when the temperature is higher than or equal to 60 DEG C is effectively solved. The environment-friendly Dacromet coating disclosed by the invention has the advantages of excellent high temperature corrosion resistance and thermal shock resistance and stable performance, a good protection function can be performed for the relevant fastener of a marine high temperature component, and the service life of the fastener can be further prolonged.
Description
Technical field
The invention belongs to material antiseptic erosion field, and in particular to a kind of high temperature resistant environment-protective Dyclo paint, coating and its
Preparation method.
Background technology
Nowadays, miscellaneous metal material has become the important substance basis of human social development, especially steel
Iron, is even more to human civilization and plays an important role.And fastener is used as the important coupling part of iron structure, its effect is more
It is to look down upon.Due to the particularity of fastener position, once it occurs corrosion, will have serious consequences.One is connection
Intensity decreases, influence the force-bearing situation of iron structure, bring very big industrial hidden danger and lead to a disaster.Two is the fastener of corrosion
Influence dismounting assembling maintenance, makes troubles.Therefore, the research to the metal parts corrosion resisting property of fastener class also becomes non-therewith
It is often important.
Conventional fastener is all made up of carbon steel and steel alloy, and for this material, its means of defence mainly has electricity
The methods such as plating, chemical plating, epoxy resin coating, oxidation processes.Wherein, the waste liquor contamination influence environment produced by electro-plating method,
Difficult treatment.Compare in this way and be not suitable for widely applying, typically only in some specific use environments, such as oil drilling
The fastener being related in platform or navigation aircraft can just use the means of defence of cadmium plating class.Nowadays metal erosion problem compared with
For it is serious in the case of, zinc-chromium coating technology has many other protection type coatings as a kind of one of preferable preventive means
Incomparable advantage, gradually the corrosion-resistant field in metal material occupy a tiny space.Zinc-chromium coating is also called Dacromet/steel,
But it is a kind of process is simple the anti-corrosion good corrosion-inhibiting coating of effect, the Technology origin is in West Automobile Enterprise industry.Process is simple, it is dirty
Metachromia is small, and corrosion resistance is good, and with certain self-repairability, these all cause that the means of defence is greatly favored.
And along with the development of modern industry, more harsh working environment is adapted to it is desirable to fastener, further open up
Open up its scope of application.Fastener such as related to ocean high-temperature pipe, descends high-temperature pipe normal working temperature in working order
During up to 100 DEG C, easily got rusty with the bolt of the traditional Dacromet/steel of coating, reason is the electricity of the main component zinc powder of Dacroment
Electrode potential will be inverted at a temperature of >=60 DEG C, and -0.12v is risen to from original -0.79v, than matrix Fe's (- 0.45v)
Electrode potential is high, therefore it loses sacrificial anode effect more than 60 DEG C, it is impossible to provide effective electrochemical protection.Thus may be used
See, although the research at present for Dacromet/steel is quite ripe, but its combination property can not fully meet reality
Industrial production demand.Such as in this extreme environment of ocean high temperature, Dacroment can not reach preferable anti-corrosion effect.Especially
Its for fastener, it as iron structure important coupling part, due to the particularity of its position, if can not be in height
Temperature is descended the certain decay resistance of holding and is suffered erosion, it will has a strong impact on the connection between metal parts, or even can bring
Very big industrial hidden danger and lead to a disaster.Further probed into it is therefore desirable to the combination property to coating, it is necessary to make coating
In high temperature, this extreme environment still possesses fabulous corrosion resisting property.
The content of the invention
The present invention is directed to the deficiencies in the prior art, it is therefore intended that provide a kind of high temperature resistant environment-protective Dacromet/steel and
Its preparation method.
For achieving the above object, the technical solution adopted in the present invention is：
A kind of high temperature resistant environment-protective Dyclo paint, each component is by weight percentage：Metal paste 45%~50%, nothing
Chromium passivating liquid 45%~50%, related auxiliaries 2%~5%.
In such scheme, the metal paste is by weight 1 by metal powder and wetting agent:1 composition.
In such scheme, the metal powder be by zinc flake, flake aluminum, sheet magnesium powder and sheet manganese powder by weight
4:1:1:1~8:1:1:1 composition.
In such scheme, the wetting agent is PEG400.
In such scheme, the chromium-free passivation liquid is by weight 1 by chrome-free tanning agent and absolute ethyl alcohol:6 compositions.
In such scheme, the chrome-free tanning agent be by ammonium molybdate, boric acid, phytic acid, silane coupler and rare earth material by
Weight compares 4：1：2：1.25：3 compositions.
In such scheme, the silane coupler is KH-560 or AC-66.
In such scheme, the rare earth material is lanthanum nitrate.
In such scheme, the related auxiliaries are by thickener, dispersant and reducing agent in mass ratio 1:1:6 compositions.
In such scheme, the thickener is hydroxymethyl cellulose, and the dispersant is OP-10, and the reducing agent is second
Glycol.
The preparation method of above-mentioned high temperature resistant environment-protective Dyclo paint, comprises the following steps：
(1) preparation of metal paste：After zinc flake, flake aluminum, sheet magnesium powder, sheet manganese powder and wetting agent are mixed
Stir, obtain metal paste；
(2) preparation of chromium-free passivation liquid：By ammonium molybdate, boric acid, phytic acid, silane coupler and rare earth material and absolute ethyl alcohol
It is well mixed, obtain chromium-free passivation liquid；
(3) preparation of related auxiliaries：Thickener, dispersant and reducing agent are well mixed, related auxiliaries are obtained；
(4) preparation of chromium-free Dyclo paint：Metal paste and chromium-free passivation liquid are added into container and is well mixed, then
Related auxiliaries are added, at room temperature 6~8h of quick stirring, the pH and viscosity of coating are controlled in whipping process；Treat pH and viscosity ginseng
After number stabilization, coating is positioned in 38 DEG C of water-baths and stands 1~1.5h, obtain chromium-free Dyclo paint.
In such scheme, the pH is 6.0~8.5, and viscosity is 20~60s, is determined to apply according to required application member size
Mode is covered, typically there is brushing, spin coating (centrifuge drying), or three kinds of modes of spraying.
In the present invention, it should be noted that concerns in the preparation process of chromium-free Dyclo paint：
1. environment should be clean dustless in proportioning room or weighing area, and under conditions of sun light direct beam is prevented, indoor light is bright
It is bright；
2. chromium-free Dyclo paint should be stored under not higher than 25 DEG C of environment temperature, and prevents periods of direct sunlight, preferably deposited
It is placed in air-conditioned room；
3. the slurry such as distilled water and coating container must use the resistant material systems such as polyethylene or polyvinyl chloride
Make.
A kind of preparation method of high temperature resistant environment-protective Dacromet/steel, comprises the following steps：
(1) base material workpiece pre-treatment：The pre-treatment of the de- ester of oil removing and rust cleaning flash removed is carried out to base material workpiece；
(2) coating, preliminary drying and sintering：High temperature resistant environment-protective Dyclo paint is coated in base material workpiece surface, workpiece table is treated
Face masking liquid is placed on 8~15min of preliminary drying at a temperature of 80~150 DEG C (caloric receptivity according to workpiece is determined) when slightly drying, make masking liquid water
Divide evaporation, levelling is uniform；Workpiece after preliminary drying is sintered 20~40min (according to workpiece at a high temperature of 300~340 DEG C
Caloric receptivity determine, it is also possible to temperature is properly increased to shorten sintering time)
(3) operation of repeat step (2) carries out second coating, preliminary drying and sintering to workpiece, and applying two by this two dries
It is prepared into high temperature resistant chromium-free Dyclo coating.
In such scheme, the base material workpiece pre-treatment comprises the following steps：
1. oil removing takes off ester：The workpiece for having oil must first carry out surface degreasing degreasing, and method is any one in following three kinds
Kind：High temperature oil removing；Water base oil-removing rust-removing agent oil removing；The Solvent degreasings such as dichloromethane, acetone, absolute ethyl alcohol；
2. eliminate rust flash removed：It is every to there is embroidery or the workpiece of burr to forbid directly to be coated, it is necessary to by the flash removed that eliminates rust
Technique, the most handy sandblasting mode of this technique is carried out, and simple acid pickling and rust removing can influence the corrosion resistance of coat and bring hydrogen embrittlement wind
Danger；Workpiece after sandblasting is placed in ultrasonic cleaning machine and cleans 30~40min with EtOH Sonicate, drying box is put into after natural air drying
In it is standby.
In such scheme, the mode point of the coating is following three kinds：Brush, spin coating (centrifuge drying), or the side for spraying
Formula carries out surface coating；General situation, the coating for fastener is carried out by the way of spin coating, is comprised the following steps that：First
Workpiece is immersed into 10~15s in chromium-free Dyclo paint, be put into get rid of in bucket just getting rid of 15 under the rotating speed of 450~550rad/s~
20s, then gets rid of 15~20s so that the rotating speed of 450~550rad/s is counter again, checks whether sample uniformly coats after having got rid of, and masking liquid is more
Place, brushed flat with hairbrush.
Beneficial effects of the present invention：Environmentally friendly Dyclo paint of the present invention substitutes part zinc powder from magnesium manganese powder, with nothing
Water-ethanol substitutes water, and the electrode potential for efficiently solving zinc powder occurs reversion at a temperature of >=60 DEG C and causes traditional Dacromet/steel
The problem of failure；Environmentally friendly Dacromet/steel of the present invention has an excellent high temperature corrosion resistance and thermal shock resistance, stable performance,
The energy pair fastener related to ocean high-temperature component plays a very good protection, and further functions as extension fastener and uses the longevity
Life.
Brief description of the drawings
Fig. 1 is temperature variation in thermal shock test of the present invention.
Fig. 2 is that workpiece carries out ammonium nitrate fast erosion experiment Front-coating mirror surface topography.
Fig. 3 is that workpiece carries out coating morphology after ammonium nitrate fast erosion experiment.
Specific embodiment
For a better understanding of the present invention, it is with reference to the embodiment content that the present invention is furture elucidated but of the invention
Content is not limited solely to the following examples.
In following examples, environmentally friendly Dacromet/steel coating needs to carry out multinomial pre-treatment to workpiece before preparing, to obtain
The erosion shield of excellent performance is obtained, to meet the need of work under the harsh environments such as high temperature, high humidity, high salt；Base material work
Part pre-treatment has following necessary step：
1) the de- ester of oil removing：The workpiece for having oil must first carry out surface degreasing degreasing, and method is any one in following three kinds
Kind：High temperature oil removing；Water base oil-removing rust-removing agent oil removing；The Solvent degreasings such as dichloromethane, acetone, absolute ethyl alcohol；
2) eliminate rust flash removed：It is every to there is embroidery or the workpiece of burr to forbid directly to be coated, it is necessary to by the flash removed that eliminates rust
Technique, the most handy sandblasting mode of this technique is carried out, and simple acid acid pickling and rust removing can influence the corrosion resistance of coat and bring hydrogen embrittlement
Risk；Workpiece after sandblasting is placed in ultrasonic cleaning machine and cleans 30~40min with EtOH Sonicate, drying is put into after natural air drying
It is standby in case.
Embodiment 1
A kind of high temperature resistant chromium-free Dyclo paint, is prepared via a method which to obtain：
(1) (wherein zinc flake, flake aluminum, sheet magnesium powder, the weight ratio of sheet manganese powder are to take the metal powder of 4.2kg
8:1:1:1) it is made metal paste with 4.2kg PEG400 mixing and stirrings；
(2) chrome-free tanning agent (wherein ammonium molybdate, boric acid, phytic acid, silane coupler KH-560, the rare earth material of 1.4kg are taken
The weight ratio of lanthanum nitrate is 4：1：2：1.25：3) and during 7kg absolute ethyl alcohols are put into container magnetic agitation is used between 30~40 DEG C
Device at the uniform velocity stirs 40~50min, you can obtain chromium-free passivation liquid；
(3) 400g related auxiliaries (wherein thickener hydroxymethyl cellulose, dispersant OP-10, the weight of reducing agent ethylene glycol are taken
Amount is than being 1:1:6) to being well mixed at room temperature in container, that is, related auxiliaries are obtained；
(4) step (1) gained metal paste, step (2) gained chromium-free passivation liquid and step (3) gained related auxiliaries are fallen
Enter and at the uniform velocity stirred after being well mixed in polyethylene drum, after 6.5 hours (now pH is 6.5, and viscosity is 46s), be positioned over 38 DEG C of water
1h is stood in bath, high temperature resistant chromium-free Dyclo paint is obtained.
Workpiece is pre-processed, 10s in the high temperature chromium-free Dyclo paint for preparing is subsequently dipped to, spin coating is put into after taking-up
15s just got rid of with 450rad/s in machine and is getting rid of 15s so that same rotating speed is counter again.It is a small amount of unnecessary that workpiece taking-up hairbrush is gently brushed away
Masking liquid, 120 DEG C of preliminary dryings 10 minutes, 30 are sintered after preliminary drying in 300 DEG C of Muffle furnaces in drying box is put into after the drying of surface masking liquid
Minute.Taking-up workpiece is coated by above-mentioned same step after sintering, preliminary drying, sintering obtain the painting of second layer chromium-free Dyclo
Layer.After applying techniques through this two baking two, high temperature resistant chromium-free Dyclo coating is finally given.With ammonium nitrate short-term corrosion test (by work
Part impregnated in the solution that ammonium nitrate mass concentration is 20wt%, and water-bath keeps 70 ± 2 DEG C of solution；Timing；Occur to matrix red
Tested during rust and terminated, terminate timing) corrosion resisting property under testing coating high temperature (before experiment with experiment after coating morphology as schemed
Shown in 2 and Fig. 3), thermal shock test (thermal shock test process is as shown in Figure 1) testing coating thermal shock resistance with metallographic microscope or is swept
Testing electronic microscope coating layer thickness is retouched, dope viscosity is tested with -4 glasss of viscosity apparatus are applied.Result is as shown in table 1, the result table of table 1
It is bright：The chromium-free Dyclo coating has excellent high temperature corrosion resistance and thermal shock resistance.
1 embodiment of table 1 prepares the performance of gained coating and coating
| The ammonium nitrate short-term corrosion test time (min) | Thermal shock number | Coating layer thickness (μm) | Apply fluid viscosity (s) |
| 143 | 328 | 10.7 | 46 |
Embodiment 2
A kind of high temperature resistant chromium-free Dyclo paint, is prepared via a method which to obtain：
(1) (wherein zinc flake, flake aluminum, sheet magnesium powder, the weight ratio of sheet manganese powder are to take the metal powder of 4.2kg
7:1:1:1) it is made metal paste with 4.2kg PEG400 mixing and stirrings；
(2) chrome-free tanning agent (wherein ammonium molybdate, boric acid, phytic acid, silane coupler KH-560, the rare earth material of 1.4kg are taken
The weight ratio of lanthanum nitrate is 4：1：2：1.25：3) and during 7kg absolute ethyl alcohols are put into container magnetic agitation is used between 30~40 DEG C
Device at the uniform velocity stirs 40~50min, you can obtain chromium-free passivation liquid；
(3) 400g related auxiliaries (wherein thickener hydroxymethyl cellulose, dispersant OP-10, the weight of reducing agent ethylene glycol are taken
Amount is than being 1:1:6) to being well mixed at room temperature in container, that is, related auxiliaries are obtained；
(4) step (1) gained metal paste, step (2) gained chromium-free passivation liquid and step (3) gained related auxiliaries are fallen
Enter and at the uniform velocity stirred after being well mixed in polyethylene drum, after 6.5 hours (now pH is 7, and viscosity is 49s), be positioned over 38 DEG C of water-baths
1h is stood in pot, high temperature resistant chromium-free Dyclo paint is obtained.
Workpiece is cleaned by ultrasonic 30 minutes with absolute ethyl alcohol, it is standby that taking-up carries out surface sand-blasting after air-drying.Workpiece is immersed
10s in the coating for preparing, is put into spin coating machine after taking-up and is just getting rid of 15s with 450rad/s and get rid of 15s so that same rotating speed is counter again.By work
Part taking-up hairbrush gently brushes away a small amount of unnecessary masking liquid, 120 DEG C of 10 points of preliminary dryings in drying box is put into after the drying of surface masking liquid
Clock, sinters 30 minutes after preliminary drying in 300 DEG C of Muffle furnaces.Workpiece is taken out after sintering to be coated by above-mentioned same step, in advance
Dry, sintering obtains second layer chromium-free Dyclo coating.After applying techniques through this two baking two, the painting of high temperature resistant chromium-free Dyclo is finally given
Layer.(workpiece be impregnated in into ammonium nitrate mass concentration in the solution of 20wt%, water-bath keeps molten with ammonium nitrate short-term corrosion test
70 ± 2 DEG C of liquid；Timing；Tested when there is red rust to matrix and terminated, terminate timing) corrosion resisting property (experiment under testing coating high temperature
Coating morphology after preceding and experiment is as shown in Figures 2 and 3), thermal shock test (thermal shock test process is as shown in Figure 1) test is applied
Layer thermal shock resistance, with metallographic microscope or scanning electron microscope test coating layer thickness, is glued with -4 glasss of viscosity apparatus test coating are applied
Degree.Result is shown in that as shown in table 2, the result of table 2 shows：The chromium-free Dyclo coating has excellent high temperature corrosion resistance and heat resistanceheat resistant
Pinking.
2 embodiment of table 2 prepares the performance of gained coating and coating
| The ammonium nitrate short-term corrosion test time (min) | Thermal shock number | Coating layer thickness (μm) | Apply fluid viscosity (s) |
| 129 | 334 | 10.5 | 49 |
Embodiment 3
A kind of high temperature resistant chromium-free Dyclo paint, is prepared via a method which to obtain：
(1) (wherein zinc flake, flake aluminum, sheet magnesium powder, the weight ratio of sheet manganese powder are to take the metal powder of 4.2kg
6:1:1:1) it is made metal paste with 4.2kg PEG400 mixing and stirrings；
(2) chrome-free tanning agent (wherein ammonium molybdate, boric acid, phytic acid, silane coupler KH-560, the rare earth material of 1.4kg are taken
The weight ratio of lanthanum nitrate is 4：1：2：1.25：3) and during 7kg absolute ethyl alcohols are put into container magnetic agitation is used between 30~40 DEG C
Device at the uniform velocity stirs 40~50min, you can obtain chromium-free passivation liquid；
(3) 400g related auxiliaries (wherein thickener hydroxymethyl cellulose, dispersant OP-10, the weight of reducing agent ethylene glycol are taken
Amount is than being 1:1:6) to being well mixed at room temperature in container, that is, related auxiliaries are obtained；
(4) step (1) gained metal paste, step (2) gained chromium-free passivation liquid and step (3) gained related auxiliaries are fallen
Enter and at the uniform velocity stirred after being well mixed in polyethylene drum, after 6.5 hours (now pH is 7, and viscosity is 54s), be positioned over 38 DEG C of water-baths
1h is stood in pot, high temperature resistant chromium-free Dyclo paint is obtained.
Workpiece is cleaned by ultrasonic 30 minutes with absolute ethyl alcohol, it is standby that taking-up carries out surface sand-blasting after air-drying.Workpiece is immersed
10s in the coating for preparing, is put into spin coating machine after taking-up and is just getting rid of 15s with 450rad/s and get rid of 15s so that same rotating speed is counter again.By work
Part taking-up hairbrush gently brushes away a small amount of unnecessary masking liquid, 120 DEG C of 10 points of preliminary dryings in drying box is put into after the drying of surface masking liquid
Clock, sinters 30 minutes after preliminary drying in 300 DEG C of Muffle furnaces.Workpiece is taken out after sintering to be coated by above-mentioned same step, in advance
Dry, sintering obtains second layer chromium-free Dyclo coating.After applying techniques through this two baking two, the painting of high temperature resistant chromium-free Dyclo is finally given
Layer.(workpiece be impregnated in into ammonium nitrate mass concentration in the solution of 20wt%, water-bath keeps molten with ammonium nitrate short-term corrosion test
70 ± 2 DEG C of liquid；Timing；Tested when there is red rust to matrix and terminated, terminate timing) corrosion resisting property (experiment under testing coating high temperature
Coating morphology after preceding and experiment is as shown in Figures 2 and 3), thermal shock test (thermal shock test process is as shown in Figure 1) test is applied
Layer thermal shock resistance, with metallographic microscope or scanning electron microscope test coating layer thickness, is glued with -4 glasss of viscosity apparatus test coating are applied
Degree.Result is shown in that as shown in table 3, the result of table 3 shows：The chromium-free Dyclo coating has excellent high temperature corrosion resistance and heat resistanceheat resistant
Pinking.
3 embodiment of table 3 prepares the performance of gained coating and coating
| The ammonium nitrate short-term corrosion test time (min) | Thermal shock number | Coating layer thickness (μm) | Apply fluid viscosity (s) |
| 114 | 334 | 10.1 | 54 |
Embodiment 4
A kind of high temperature resistant chromium-free Dyclo paint, is prepared via a method which to obtain：
(1) (wherein zinc flake, flake aluminum, sheet magnesium powder, the weight ratio of sheet manganese powder are to take the metal powder of 4.2kg
5:1:1:1) it is made metal paste with 4.2kg PEG400 mixing and stirrings；
(2) chrome-free tanning agent (wherein ammonium molybdate, boric acid, phytic acid, silane coupler KH-560, the rare earth material of 1.4kg are taken
The weight ratio of lanthanum nitrate is 4：1：2：1.25：3) and during 7kg absolute ethyl alcohols are put into container magnetic agitation is used between 30~40 DEG C
Device at the uniform velocity stirs 40~50min, you can obtain chromium-free passivation liquid；
(3) 400g related auxiliaries (wherein thickener hydroxymethyl cellulose, dispersant OP-10, the weight of reducing agent ethylene glycol are taken
Amount is than being 1:1:6) to being well mixed at room temperature in container, that is, related auxiliaries are obtained；
(4) step (1) gained metal paste, step (2) gained chromium-free passivation liquid and step (3) gained related auxiliaries are fallen
Enter and at the uniform velocity stirred after being well mixed in polyethylene drum, after 6.5 hours (now pH is 6, and viscosity is 49s), be positioned over 38 DEG C of water-baths
1h is stood in pot, high temperature resistant chromium-free Dyclo paint is obtained.
Workpiece is cleaned by ultrasonic 30 minutes with absolute ethyl alcohol, it is standby that taking-up carries out surface sand-blasting after air-drying.Workpiece is immersed
10s in the coating for preparing, is put into spin coating machine after taking-up and is just getting rid of 15s with 450rad/s and get rid of 15s so that same rotating speed is counter again.By work
Part taking-up hairbrush gently brushes away a small amount of unnecessary masking liquid, 120 DEG C of 10 points of preliminary dryings in drying box is put into after the drying of surface masking liquid
Clock, sinters 30 minutes after preliminary drying in 300 DEG C of Muffle furnaces.Workpiece is taken out after sintering to be coated by above-mentioned same step, in advance
Dry, sintering obtains second layer chromium-free Dyclo coating.After applying techniques through this two baking two, the painting of high temperature resistant chromium-free Dyclo is finally given
Layer.(workpiece be impregnated in into ammonium nitrate mass concentration in the solution of 20wt%, water-bath keeps molten with ammonium nitrate short-term corrosion test
70 ± 2 DEG C of liquid；Timing；Tested when there is red rust to matrix and terminated, terminate timing) corrosion resisting property (experiment under testing coating high temperature
Coating morphology after preceding and experiment is as shown in Figures 2 and 3), thermal shock test (thermal shock test process is as shown in Figure 1) test is applied
Layer thermal shock resistance, with metallographic microscope or scanning electron microscope test coating layer thickness, is glued with -4 glasss of viscosity apparatus test coating are applied
Degree.Result is shown in that as shown in table 4, the result of table 4 shows：The chromium-free Dyclo coating has excellent high temperature corrosion resistance and heat resistanceheat resistant
Pinking.
4 embodiment of table 4 prepares the performance of gained coating and coating
| The ammonium nitrate short-term corrosion test time (min) | Thermal shock number | Coating layer thickness (μm) | Apply fluid viscosity (s) |
| 132 | 347 | 9.9 | 49 |
Embodiment 5
A kind of high temperature resistant chromium-free Dyclo paint, is prepared via a method which to obtain：
(1) (wherein zinc flake, flake aluminum, sheet magnesium powder, the weight ratio of sheet manganese powder are to take the metal powder of 4.2kg
4:1:1:1) it is made metal paste with 4.2kg PEG400 mixing and stirrings；
(2) chrome-free tanning agent (wherein ammonium molybdate, boric acid, phytic acid, silane coupler KH-560, the rare earth material of 1.4kg are taken
The weight ratio of lanthanum nitrate is 4：1：2：1.25：3) and during 7kg absolute ethyl alcohols are put into container magnetic agitation is used between 30~40 DEG C
Device at the uniform velocity stirs 40~50min, you can obtain chromium-free passivation liquid；
(3) 400g related auxiliaries (wherein thickener hydroxymethyl cellulose, dispersant OP-10, the weight of reducing agent ethylene glycol are taken
Amount is than being 1:1:6) to being well mixed at room temperature in container, that is, related auxiliaries are obtained；
(4) step (1) gained metal paste, step (2) gained chromium-free passivation liquid and step (3) gained related auxiliaries are fallen
Enter and at the uniform velocity stirred after being well mixed in polyethylene drum, after 6.5 hours (now pH is 6.5, and viscosity is 52s), be positioned over 38 DEG C of water
1h is stood in bath, high temperature resistant chromium-free Dyclo paint is obtained.
Workpiece is cleaned by ultrasonic 30 minutes with absolute ethyl alcohol, it is standby that taking-up carries out surface sand-blasting after air-drying.Workpiece is immersed
10s in the coating for preparing, is put into spin coating machine after taking-up and is just getting rid of 15s with 450rad/s and get rid of 15s so that same rotating speed is counter again.By work
Part taking-up hairbrush gently brushes away a small amount of unnecessary masking liquid, 120 DEG C of 10 points of preliminary dryings in drying box is put into after the drying of surface masking liquid
Clock, sinters 30 minutes after preliminary drying in 300 DEG C of Muffle furnaces.Workpiece is taken out after sintering to be coated by above-mentioned same step, in advance
Dry, sintering obtains second layer chromium-free Dyclo coating.After applying techniques through this two baking two, the painting of high temperature resistant chromium-free Dyclo is finally given
Layer.(workpiece be impregnated in into ammonium nitrate mass concentration in the solution of 20wt%, water-bath keeps molten with ammonium nitrate short-term corrosion test
70 ± 2 DEG C of liquid；Timing；Tested when there is red rust to matrix and terminated, terminate timing) corrosion resisting property (experiment under testing coating high temperature
Coating morphology after preceding and experiment is as shown in Figures 2 and 3), thermal shock test (thermal shock test process is as shown in Figure 1) test is applied
Layer thermal shock resistance, with metallographic microscope or scanning electron microscope test coating layer thickness, is glued with -4 glasss of viscosity apparatus test coating are applied
Degree.Result is shown in that as shown in table 5, the result of table 5 shows：The chromium-free Dyclo coating has excellent high temperature corrosion resistance and heat resistanceheat resistant
Pinking.
5 embodiment of table 5 prepares the performance of gained coating and coating
| The ammonium nitrate short-term corrosion test time (min) | Thermal shock number | Coating layer thickness (μm) | Apply fluid viscosity (s) |
| 162 | 357 | 10.3 | 52 |
Obviously, above-described embodiment is only intended to clearly illustrate made example, and not to the limitation of implementation method.It is right
For those of ordinary skill in the art, can also make on the basis of the above description other multi-forms change or
Change.There is no need and unable to be exhaustive to all of implementation method.And the obvious change or change therefore amplified
Move within still in the protection domain of the invention.
Claims (10)
1. a kind of high temperature resistant environment-protective Dyclo paint, it is characterised in that each component is by weight percentage：Metal paste
45% ~ 50%, chromium-free passivation liquid 45% ~ 50%, related auxiliaries 2% ~ 5%.
2. high temperature resistant environment-protective Dyclo paint according to claim 1, it is characterised in that the metal paste is by metal powder
With
Wetting agent is by weight 1：1 composition.
3. high temperature resistant environment-protective Dyclo paint according to claim 2, it is characterised in that the metal powder is by sheet zinc
Powder,
Flake aluminum, sheet magnesium powder and sheet manganese powder are by weight 4：1：1：1~8：1：1：1 composition.
4. high temperature resistant environment-protective Dyclo paint according to claim 2, it is characterised in that the wetting agent is polyethylene glycol
400。
5. high temperature resistant environment-protective Dyclo paint according to claim 1, it is characterised in that the chromium-free passivation liquid is by Chrome-free
It is blunt
Agent and absolute ethyl alcohol are by weight 1：6 compositions.
6. high temperature resistant environment-protective Dyclo paint according to claim 5, it is characterised in that the chrome-free tanning agent is by molybdic acid
Ammonium,
Boric acid, phytic acid, silane coupler and rare earth material are by weight 4：1：2：1.25：3 compositions.
7. high temperature resistant environment-protective Dyclo paint according to claim 6, it is characterised in that the silane coupler is KH-560
Or
AC-66；The rare earth material is lanthanum nitrate.
8. high temperature resistant environment-protective Dyclo paint according to claim 1, it is characterised in that the related auxiliaries are by thickening
Agent,
Dispersant and reducing agent in mass ratio 1：1：6 compositions.
9. the preparation method of any high temperature resistant environment-protective Dyclo paint of claim 1 ~ 8, it is characterised in that including following step
Suddenly：
（1）The preparation of metal paste：Stirred after zinc flake, flake aluminum, sheet magnesium powder, sheet manganese powder and wetting agent are mixed
Uniformly, metal paste is obtained；
（2）The preparation of chromium-free passivation liquid：Ammonium molybdate, boric acid, phytic acid, silane coupler and rare earth material and absolute ethyl alcohol are mixed
Uniformly, chromium-free passivation liquid is obtained；
（3）The preparation of related auxiliaries：Thickener, dispersant and reducing agent are well mixed, related auxiliaries are obtained；
（4）The preparation of chromium-free Dyclo paint：Metal paste and chromium-free passivation liquid are added into container and is well mixed, added
Related auxiliaries, 6 ~ 8h of quick stirring, controls the pH and viscosity of coating at room temperature in whipping process；Treat pH and viscosity parameter stabilization
Afterwards, coating is positioned in 38 DEG C of water-baths and stands 1 ~ 1.5h, obtain chromium-free Dyclo paint.
10. it is a kind of to prepare the painting of high temperature resistant environment-protective Dacroment using any high temperature resistant environment-protective Dyclo paint of claim 1 ~ 8
The side of layer
Method, it is characterised in that comprise the following steps：
（1）Base material workpiece pre-treatment：The pre-treatment of the de- ester of oil removing and rust cleaning flash removed is carried out to base material workpiece；
（2）Coating, preliminary drying and sintering：High temperature resistant environment-protective Dyclo paint is coated in base material workpiece surface, treats that workpiece surface is applied
8 ~ 15min of preliminary drying at a temperature of 80 ~ 150 DEG C are placed on when liquid is slightly dried, makes masking liquid moisture evaporation, and levelling is uniform；After preliminary drying
Workpiece is sintered 20 ~ 40min at a high temperature of 300 ~ 340 DEG C；
（3）Repeat step（2）Operation second coating, preliminary drying and sintering are carried out to workpiece, by this two apply two bake it is standby
Obtain high temperature resistant chromium-free Dyclo coating.
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