CN110452599A - Protective coating and preparation method thereof for differential arc oxidation - Google Patents
Protective coating and preparation method thereof for differential arc oxidation Download PDFInfo
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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
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Abstract
The invention discloses the protective coatings and preparation method thereof for differential arc oxidation, firstly, preparing binder resin;Modified organic silicone resin is prepared again;Above-mentioned binder resin is added in movable tank, modified organic silicone resin, fire retardant, fumed silica, dimethicone, defoaming agent, mill base and solvent is sequentially added and is mixed, it is stirred evenly using high-speed mixer, obtains mixed material;Mixed material is ground using sand mill, until the fineness of mixed material reaches 30 μm hereinafter, obtaining the protective coating for differential arc oxidation.Protective coating prepared by the present invention for differential arc oxidation has and solidifies at low temperature, acid and alkali resistance good to valve metal and its alloy adhesive force, and has the characteristics that in differential arc oxidation process good protection, and simple process, at low cost.
Description
Technical field
The invention belongs to differential arc oxidation film layer protection technology field, it is related to the protective coating for differential arc oxidation, the present invention
Further relate to the preparation method of above-mentioned coating.
Background technique
Differential arc oxidation (MAO-Microarc Oxidation), be it is a kind of in valve metals such as aluminium, magnesium, titanium, zirconium, tantalum, niobiums and
The new technology of its alloy surface growth in situ ceramic layer.There is hardness using ceramic film of the technology prepared by metal surface
The excellent overall characteristics such as high, wear-resisting, anti-corrosion, insulation, are widely used in Aeronautics and Astronautics, navigation, machinery, electronics, decoration, friendship
The fields such as logical, weaving.
Micro-arc oxidation ceramic layer has insulation characterisitic, and many many electronic products are gone back while requiring anti-corrosion, wear-resisting
It needs that there is conductive characteristic in regional area, so need to carry out at protection localised region of conductivity in differential arc oxidation process
Reason.In addition, because differential arc oxidation film layer is mainly to outgrowth, axis higher for some size matching requirements precision or hole class dress
It is also required to carry out protection processing with face.Therefore, the localised protection mode of micro-arc oxidation treatment is the urgency faced in production process
Problem to be solved.There is oxidation breakdown voltage height in micro-arc oxidation process, (aluminium alloy voltage is up to 650V or more), solution
The features such as in weak base or strong basicity, shelf depreciation spark temperature high (about 2000 DEG C or more), so that using traditional anodic oxidation
Or electroplating protecting coating is unable to satisfy requirement, and when using production tooling protection there are process-cycle length, overprotection,
The problems such as at high cost.
Summary of the invention
The object of the present invention is to provide the protective coating for differential arc oxidation, have and solidify at low temperature, to valve metal and
Its alloy adhesive force is good, acid and alkali resistance, and has the characteristics that well to protect in differential arc oxidation process.
It is a further object of the present invention to provide the preparation method for above-mentioned protective coating, there is simple process, at low cost,
And the characteristics of differential arc oxidation film layer is easily peeled off.
A kind of technical solution of the present invention is, for the protective coating of differential arc oxidation, according to mass percent by
Following raw material components:
Binder resin 44%~48%, modified organic silicone resin 6%~8%, fire retardant 6%~8%, fumed silica
2.7%~4.0%, dimethicone 0.3%~0.6%, defoaming agent 0.3%~0.8%, mill base 1.5%~2.5%, remaining
For solvent.
The features of the present invention also characterized in that:
Binder resin is made of polyisobutene, SBS resin and solvent, the mass percent of polyisobutene is 6%~15%,
The mass percent of SBS resin is 15%~20%, and surplus is solvent;Solvent is dimethyl carbonate and butyl acetate.
Modified organic silicone resin includes dialkyl polydimethylsiloxane and silane coupling agent;Dihydroxy polydimethyl silicon oxygen
The mass percent of alkane is 95%~98%, and the mass percent of silane coupling agent is 2%~5%;
The viscosity of dialkyl polydimethylsiloxane is 3000~10000mPa.S;Silane coupling agent is amino silane coupling
Any one in agent, vinyl silicane coupling agent, acryloxy silane coupling agent and epoxy silane coupling.
Fire retardant be zinc borate, antimony oxide, magnesium hydroxide and expansile graphite in any one or it is two kinds any
The mixture of compounding.
The partial size of fumed silica is 25~50nm.
The viscosity of dimethicone is 100~1000mPa.S.
Defoaming agent is any one in BYK-085, BYK-060N.
Mill base is made of kaolin, blanc fixe and cobalt titanate green;Kaolinic mass percent be 63.60%~
73.42%, the mass percent of blanc fixe is 26.54%~36.39%, the mass percent of the green cobalt of titanium is 0.01%~
0.04%
Solvent is any one in tetrachloro-ethylene, dimethylbenzene, dimethyl carbonate and butyl acetate.
Another technical solution adopted in the present invention is that the preparation method of the protective coating for differential arc oxidation, specifically
It follows the steps below to implement:
Step 1 prepares binder resin
It is respective that mass percent is that 6%~15% polyisobutene and 15%~20% SBS resin pour into respectively
Reaction kettle, and it is separately added into dimethyl carbonate and butyl acetate is impregnated, stirring obtains binder resin to being uniformly mixed, standby
With;
Step 2 prepares modified organic silicone resin
It is 95%~98% dialkyl polydimethylsiloxane and 2%~5% silane coupling agent by mass percent
It is down to room temperature after mixing 30~120min under 60~120 DEG C, the vacuum condition of -0.09~-0.1MPa, obtains modified organic silicon
Resin, it is spare;
The binder resin that mass percent is 44%~48% is added in movable tank step 3, sequentially adds quality hundred
Score be 6%~8% modified organic silicone resin, 6%~8% fire retardant, 2.7%~4.0% fumed silica,
0.3%~0.6% dimethicone, 0.3%~0.8% defoaming agent, 1.5%~2.5% mill base, remaining be solvent,
It is mixed, it is stirred evenly using high-speed mixer, obtains mixed material;
Step 4 grinds mixed material using sand mill, using Hegman grind gage to the mixed material after grinding into
Row test, until its fineness reaches 30 μm hereinafter, obtaining the protective coating for differential arc oxidation.
The beneficial effects of the present invention are:
(1), the present invention is used for the protective coating of differential arc oxidation, has and solidifies at low temperature, attached to valve metal and its alloy
Put forth effort, acid and alkali resistance the characteristics of;By the way that improved organic siliconresin is added, effectively increase peelable glue and aluminium, magnesium, titanium and
The adhesive strength of its alloy base material;Fire retardant, which is added, carbonization phenomenon occurs to avoid the edge of protective coating;Gas phase two is added
Silica increases the leakproofness and barrier properties of product;Dimethicone, which is added, makes protective coating have good rippability;
When using protective coating of the invention that can meet oxidated layer thickness for 50 μm or more, and the neat in edge of protective coating is consistent, nothing
Leakage phenomenon.
(2), the present invention prepares the protective coating for differential arc oxidation, extends the multifunctionality of protective coating, more can
Meets the needs of practical application, the practical application for reinforcing protective coating is of great significance;The present invention is used for differential arc oxidation
Protective coating preparation method, it is simple process, at low cost.
Specific embodiment
The present invention is described in detail With reference to embodiment.
The present invention relates to a kind of protective coatings for differential arc oxidation, according to mass percent by following raw material components:
Binder resin 44%~48%, modified organic silicone resin 6%~8%, fire retardant 6%~8%, fumed silica
2.7%~4.0%, dimethicone 0.3%~0.6%, defoaming agent 0.3%~0.8%, mill base 1.5%~2.5%, remaining
For solvent.
Binder resin is made of polyisobutene, SBS resin, and the mass percent of polyisobutene is 6%~15%, SBS tree
The mass percent of rouge is 15%~20%, and surplus is solvent;Solvent is dimethyl carbonate and butyl acetate.
Modified organic silicone resin includes dialkyl polydimethylsiloxane and silane coupling agent;Dihydroxy polydimethyl silicon oxygen
The mass percent of alkane is 95%~98%, and the mass percent of silane coupling agent is 2%~5%;
The viscosity of dialkyl polydimethylsiloxane is 3000~10000mPa.S;Silane coupling agent is amino silane coupling
Any one in agent, vinyl silicane coupling agent, acryloxy silane coupling agent and epoxy silane coupling.
Fire retardant be zinc borate, antimony oxide, magnesium hydroxide and expansile graphite in any one or it is two kinds any
The mixture of compounding.
The partial size of fumed silica is 25~50nm.
The viscosity of dimethicone is 100~1000mPa.S.
Defoaming agent is any one in BYK-085, BYK-060N.
Mill base is made of kaolin, blanc fixe and cobalt titanate green;Kaolinic mass percent be 63.60%~
73.42%, the mass percent of blanc fixe is 26.54%~36.39%, the mass percent of the green cobalt of titanium is 0.01%~
0.04%
Solvent is any one in tetrachloro-ethylene, dimethylbenzene, dimethyl carbonate and butyl acetate.
The invention further relates to the preparation methods of the protective coating for differential arc oxidation, are specifically implemented according to the following steps:
Step 1 prepares binder resin
It is respective that mass percent is that 6%~15% polyisobutene and 15%~20% SBS resin pour into respectively
Reaction kettle, and it is separately added into dimethyl carbonate and butyl acetate is impregnated, stirring obtains binder resin to being uniformly mixed, standby
With;
Step 2 prepares modified organic silicone resin
It is 95%~98% dialkyl polydimethylsiloxane and 2%~5% silane coupling agent by mass percent
It is down to room temperature after mixing 30~120min under 60~120 DEG C, the vacuum condition of -0.09~-0.1MPa, obtains modified organic silicon
Resin, it is spare;
The binder resin that mass percent is 44%~48% is added in movable tank step 3, sequentially adds quality hundred
Score be 6%~8% modified organic silicone resin, 6%~8% fire retardant, 2.7%~4.0% fumed silica,
0.3%~0.6% dimethicone, 0.3%~0.8% defoaming agent, 1.5%~2.5% mill base, remaining be solvent,
It is mixed, it is stirred evenly using high-speed mixer, obtains mixed material;
Step 4 grinds mixed material using sand mill, using Hegman grind gage to the mixed material after grinding into
Row test, until its fineness reaches 30 μm hereinafter, obtaining the protective coating for differential arc oxidation.
Embodiment 1
(1) binder resin is prepared
It is that 6% polyisobutene and 15% SBS resin pour into respective reaction kettle, and difference respectively by mass percent
34% dimethyl carbonate is added and 45% butyl acetate is impregnated, stirring obtains binder resin to being uniformly mixed, standby
With;
(2) modified organic silicone resin is prepared
By mass percent be 98% dialkyl polydimethylsiloxane and 2% silane coupling agent 80 DEG C ,-
It is down to room temperature after mixing 60min under the vacuum condition of 0.1MPa, obtains modified organic silicone resin, it is spare;
Wherein, the viscosity of dialkyl polydimethylsiloxane is 5000mPa.S;Silane coupling agent is amino silane coupling
Agent.
(3) binder resin that mass percent is 44% is added in movable tank, sequentially adds 8% modified organic silicon
Resin, 8% fire retardant, 2.7% fumed silica, 0.6% dimethicone, 0.3% defoaming agent, 1.5%
Mill base and 34.9% solvent are mixed, and are stirred evenly using high-speed mixer to it, are obtained mixed material;
Wherein, the revolving speed of high-speed mixer is 2000 turns/min;Fire retardant is zinc borate, and the partial size of fumed silica is
25nm, the viscosity of dimethicone are 200mPa.S, defoaming agent BYK-085, mill base group as 65% kaolin,
34.98% blanc fixe and 0.02% the green cobalt of titanium, solvent is tetrachloro-ethylene.
(4) mixed material is ground using sand mill, the mixed material after grinding is carried out using Hegman grind gage
Test, until the fineness of mixed material reaches 30 μm hereinafter, obtaining the protective coating for differential arc oxidation.
Embodiment 2,
(1) binder resin is prepared
It is that 8% polyisobutene and 20% SBS resin pour into respective reaction kettle, and difference respectively by mass percent
30% dimethyl carbonate is added and 42% butyl acetate is impregnated, stirring obtains binder resin to being uniformly mixed, standby
With;
(2) modified organic silicone resin is prepared
By mass percent be 95% dialkyl polydimethylsiloxane and 5% silane coupling agent 120 DEG C ,-
It is down to room temperature after mixing 30min under the vacuum condition of 0.09MPa, obtains modified organic silicone resin, it is spare;
Wherein, the viscosity of dialkyl polydimethylsiloxane is 8000mPa.S;Silane coupling agent is vinyl silanes coupling
Agent.
(3) binder resin that mass percent is 48% is added in movable tank, sequentially adds 6% modified organic silicon
Resin, 7% fire retardant, 3% fumed silica, 0.3% dimethicone, 0.4% defoaming agent, 2% mill base
Solvent with 33.3% is mixed, and is stirred evenly using high-speed mixer to it, is obtained mixed material;
Wherein, the revolving speed of high-speed mixer is 2000 turns/min;Fire retardant is magnesium hydroxide, the partial size of fumed silica
For 40nm, the viscosity of dimethicone is 500mPa.S, defoaming agent BYK-060N, mill base group as 70% kaolin,
29.96% blanc fixe and 0.04% the green cobalt of titanium, solvent is dimethylbenzene.
(4) mixed material is ground using sand mill, the mixed material after grinding is carried out using Hegman grind gage
Test, until the fineness of mixed material reaches 30 μm hereinafter, obtaining the protective coating for differential arc oxidation.
Embodiment 3,
(1) binder resin is prepared
It is that 7% polyisobutene and 18% SBS resin pour into respective reaction kettle, and difference respectively by mass percent
32% dimethyl carbonate is added and 43% butyl acetate is impregnated, stirring obtains binder resin to being uniformly mixed, standby
With;
(2) modified organic silicone resin is prepared
By mass percent be 96% dialkyl polydimethylsiloxane and 4% silane coupling agent 100 DEG C ,-
It is down to room temperature after mixing 40min under the vacuum condition of 0.09MPa, obtains modified organic silicone resin, it is spare;
Wherein, the viscosity of dialkyl polydimethylsiloxane is 10000mPa.S;Silane coupling agent is propiono oxygroup silicon
Oxygen alkane.
(3) binder resin that mass percent is 46% is added in movable tank, sequentially adds 7% modified organic silicon
Resin, 8% fire retardant, 3.6% fumed silica, 0.45% dimethicone, 0.5% defoaming agent, 1.8%
Mill base and 32.65% solvent are mixed, and are stirred evenly using high-speed mixer to it, are obtained mixed material;
Wherein, the revolving speed of high-speed mixer is 2000 turns/min;Fire retardant is the dilatancy stone that mass percent is 60%
Ink and 40% antimony oxide, the partial size of fumed silica is 50nm, and the viscosity of dimethicone is 1000mPa.S, is disappeared
Infusion is BYK-085, mill base group become 66% kaolin, 33.97% blanc fixe and 0.03% the green cobalt of titanium, solvent
For dimethyl carbonate.
(4) mixed material is ground using sand mill, the mixed material after grinding is carried out using Hegman grind gage
Test, until the fineness of mixed material reaches 30 μm hereinafter, obtaining the protective coating for differential arc oxidation.
Embodiment 4
(1) binder resin is prepared
It is that 6% polyisobutene and 19% SBS resin pour into respective reaction kettle, and difference respectively by mass percent
31.5% dimethyl carbonate is added and 43.5% butyl acetate is impregnated, stirring obtains binder resin to being uniformly mixed,
It is spare;
(2) modified organic silicone resin is prepared
By mass percent be 95.5% dialkyl polydimethylsiloxane and 4.5% silane coupling agent 60 DEG C ,-
It is down to room temperature after mixing 120min under the vacuum condition of 0.09MPa, obtains modified organic silicone resin, it is spare;
Wherein, the viscosity of dialkyl polydimethylsiloxane is 7000mPa.S;Silane coupling agent is epoxy radicals silicone hydride coupling
Agent.
(3) binder resin that mass percent is 45% is added in movable tank, sequentially adds 8% modified organic silicon
Resin, 7% fire retardant, 3% fumed silica, 0.5% dimethicone, 0.8% defoaming agent, 2.5% color
It starches and 33.2% solvent is mixed, it is stirred evenly using high-speed mixer, obtains mixed material;
Wherein, the revolving speed of high-speed mixer is 2000 turns/min;Fire retardant is zinc borate, and the partial size of fumed silica is
30nm, the viscosity of dimethicone are 100mPa.S, defoaming agent BYK-060N, mill base group as 68% kaolin,
31.95% blanc fixe and 0.05% the green cobalt of titanium, solvent is butyl acetate.
(4) mixed material is ground using sand mill, the mixed material after grinding is carried out using Hegman grind gage
Test, until the fineness of mixed material reaches 30 μm hereinafter, obtaining the protective coating for differential arc oxidation.
Embodiment 5
(1) binder resin is prepared
Mass percent is poured into respective reaction kettle for 7.5% polyisobutene and 19.5% SBS resin respectively, and
It being separately added into 33% dimethyl carbonate and 40% butyl acetate is impregnated, stirring obtains binder resin to being uniformly mixed,
It is spare;
(2) modified organic silicone resin is prepared
It is 97.5% dialkyl polydimethylsiloxane and 2.5% silane coupling agent 110 by mass percent
DEG C, mix 50min under the vacuum condition of -0.1MPa after be down to room temperature, obtain modified organic silicone resin, it is spare;
Wherein, the viscosity of dialkyl polydimethylsiloxane is 5000mPa.S;Silane coupling agent is vinyl silanes coupling
Agent.
(3) mass percent is organic for the modification in 47% binder resin addition movable tank, sequentially adding 7.5%
Silicone resin, 6% fire retardant, 4% fumed silica, 0.35% dimethicone, 0.6% defoaming agent, 2.2%
Mill base and 32.35% solvent are mixed, and are stirred evenly using high-speed mixer to it, are obtained mixed material;
Wherein, the revolving speed of high-speed mixer is 2000 turns/min;Fire retardant is zinc borate, and the partial size of fumed silica is
50nm, the viscosity of dimethicone are 500mPa.S, defoaming agent BYK-060N, mill base group as 65% kaolin,
34.95% blanc fixe and 0.05% the green cobalt of titanium, solvent is dimethylbenzene.
(4) mixed material is ground using sand mill, the mixed material after grinding is carried out using Hegman grind gage
Test, until the fineness of mixed material reaches 30 μm hereinafter, obtaining the protective coating for differential arc oxidation.
It is as shown in table 1 to the performance test of the protective coating for differential arc oxidation of Examples 1 to 5 preparation.
Performance test in table 1, Examples 1 to 5 for the protective coating of differential arc oxidation
As it can be seen from table 1 being directed to distinctive high-tension phenomena in differential arc oxidation process, silicon is introduced in the present invention
Oxygen alkane resin can effectively improve the hole breakdown capability of protective coating;A small amount of silane coupling agent is added to be modified siloxanes
Afterwards, the bond strength between protective coating and matrix can be improved;Suitable dimethicone purpose is added to be to protect completion
Afterwards, it is easy to remove protective coating from matrix;Suitable fire retardant, which is added, to be gone out to avoid protective coating and substrate intersection
The existing carbonization phenomenon for causing edge to occur because of the local spark generated in micro-arc oxidation process;Fumed silica is added to increase
The leakproofness and barrier properties of product;Defoaming agent, which is added, to be caused to avoid the bubble that protective coating generates during the drying process
Product generates leakage protection at intermediate especially turning position;The purpose that mill base is added is to distinguish the face of protective coating and substrate
Color, to be easy to check and then remove the coating of overprotection in actual operation.
Claims (10)
1. being used for the protective coating of differential arc oxidation, which is characterized in that according to mass percent by following raw material components:
Binder resin 44%~48%, modified organic silicone resin 6%~8%, fire retardant 6%~8%, fumed silica
2.7%~4.0%, dimethicone 0.3%~0.6%, defoaming agent 0.3%~0.8%, mill base 1.5%~2.5%, remaining
For solvent.
2. being used for the protective coating of differential arc oxidation as described in claim 1, which is characterized in that the binder resin is by poly- isobutyl
Alkene, SBS resin and solvent composition, the mass percent of the polyisobutene are the quality hundred of 6%~15%, the SBS resin
Divide than being 15%~20%, surplus is solvent;The solvent is dimethyl carbonate and butyl acetate.
3. being used for the protective coating of differential arc oxidation as described in claim 1, which is characterized in that the modified organic silicone resin packet
Include dialkyl polydimethylsiloxane and silane coupling agent;The mass percent of the dialkyl polydimethylsiloxane is 95%
~98%, the mass percent of the silane coupling agent is 2%~5%;
The viscosity of the dialkyl polydimethylsiloxane is 3000~10000mPa.S;The silane coupling agent is amino silane
Any one in coupling agent, vinyl silicane coupling agent, acryloxy silane coupling agent and epoxy silane coupling.
4. as described in claim 1 be used for differential arc oxidation protective coating, which is characterized in that the fire retardant be zinc borate,
Any one in antimony oxide, magnesium hydroxide and expansile graphite or any two kinds of mixtures compounded.
5. being used for the protective coating of differential arc oxidation as described in claim 1, which is characterized in that the grain of the fumed silica
Diameter is 25~50nm.
6. being used for the protective coating of differential arc oxidation as described in claim 1, which is characterized in that the viscosity of the dimethicone
For 100~1000mPa.S.
7. as described in claim 1 be used for differential arc oxidation protective coating, which is characterized in that the defoaming agent be BYK-085,
Any one in BYK-060N.
8. being used for the protective coating of differential arc oxidation as described in claim 1, which is characterized in that the mill base is by kaolin, heavy
Shallow lake barium sulfate and cobalt titanate green composition;The kaolinic mass percent is 63.60%~73.42%, the blanc fixe
Mass percent be 26.54%~36.39%, the mass percent of the green cobalt of titanium is 0.01%~0.04%.
9. as described in claim 1 be used for differential arc oxidation protective coating, which is characterized in that the solvent be tetrachloro-ethylene,
Any one in dimethylbenzene, dimethyl carbonate and butyl acetate.
10. the preparation method for the protective coating of differential arc oxidation, feature exist as claimed in any one of claims 1 to 9 wherein
In being specifically implemented according to the following steps:
Step 1 prepares binder resin
It is that 6%~15% polyisobutene and 15%~20% SBS resin pour into respective reaction respectively by mass percent
Kettle, and it is separately added into dimethyl carbonate and butyl acetate is impregnated, stirring obtains binder resin to being uniformly mixed, spare;
Step 2 prepares modified organic silicone resin
It is 95%~98% dialkyl polydimethylsiloxane and 2%~5% silane coupling agent 60 by mass percent
~120 DEG C, mix 30~120min under the vacuum condition of -0.09~-0.1MPa after be down to room temperature, obtain modified organic silicon tree
Rouge, it is spare;
The binder resin that mass percent is 44%~48% is added in movable tank step 3, sequentially adds quality hundred
Score be 6%~8% modified organic silicone resin, 6%~8% fire retardant, 2.7%~4.0% the gas
Aerosil, 0.3%~0.6% dimethicone, 0.3%~0.8% defoaming agent, 1.5%~2.5%
The mill base, remaining is solvent, is mixed, and is stirred evenly using high-speed mixer to it, obtains mixed material;
Step 4 grinds the mixed material using sand mill, using Hegman grind gage to the mixed material after grinding into
Row test, until its fineness reaches 30 μm hereinafter, obtaining the protective coating for being used for differential arc oxidation.
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