CN110452599B - Protective coating for micro-arc oxidation and preparation method thereof - Google Patents

Protective coating for micro-arc oxidation and preparation method thereof Download PDF

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CN110452599B
CN110452599B CN201910816329.8A CN201910816329A CN110452599B CN 110452599 B CN110452599 B CN 110452599B CN 201910816329 A CN201910816329 A CN 201910816329A CN 110452599 B CN110452599 B CN 110452599B
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protective coating
arc oxidation
coupling agent
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CN110452599A (en
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陈鼎
李均明
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Xi'an Qiangwei Electric Equipment Co ltd
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    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING 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
    • C09D153/00Coating compositions based on block copolymers containing at least one sequence of a polymer obtained by reactions only involving carbon-to-carbon unsaturated bonds; Coating compositions based on derivatives of such polymers
    • C09D153/02Vinyl aromatic monomers and conjugated dienes
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING 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
    • C09D5/00Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/20Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes for coatings strippable as coherent films, e.g. temporary coatings strippable as coherent films
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING 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
    • C09D7/00Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40Additives
    • C09D7/60Additives non-macromolecular
    • C09D7/61Additives non-macromolecular inorganic
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    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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    • C09D7/00Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40Additives
    • C09D7/70Additives characterised by shape, e.g. fibres, flakes or microspheres
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • C08K2003/2217Oxides; Hydroxides of metals of magnesium
    • C08K2003/2224Magnesium hydroxide
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/30Sulfur-, selenium- or tellurium-containing compounds
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
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    • C08K3/38Boron-containing compounds
    • C08K2003/387Borates
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/02Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
    • C08L2205/025Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/03Polymer mixtures characterised by other features containing three or more polymers in a blend
    • C08L2205/035Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend

Abstract

The invention discloses a protective coating for micro-arc oxidation and a preparation method thereof, and the protective coating comprises the following steps of firstly, preparing base resin; then preparing modified organic silicon resin; adding the base resin into a movable tank, sequentially adding the modified organic silicon resin, the flame retardant, the fumed silica, the dimethyl silicon oil, the defoaming agent, the color paste and the solvent for mixing, and uniformly stirring by using a high-speed stirrer to obtain a mixed material; and grinding the mixed material by using a sand mill until the fineness of the mixed material reaches below 30 mu m to obtain the protective coating for micro-arc oxidation. The protective coating for micro-arc oxidation prepared by the invention has the characteristics of low-temperature curing, good adhesion to valve metal and alloy thereof, acid and alkali resistance, good protection in the micro-arc oxidation processing process, simple process and low cost.

Description

Protective coating for micro-arc oxidation and preparation method thereof
Technical Field
The invention belongs to the technical field of micro-arc oxidation film layer protection, relates to a protective coating for micro-arc oxidation, and further relates to a preparation method of the coating.
Background
Micro-arc Oxidation (MAO-micro Oxidation) is a new technology for growing ceramic layers in situ on the surfaces of valve metals such as aluminum, magnesium, titanium, zirconium, tantalum, niobium and the like and alloys thereof. The ceramic film prepared on the metal surface by adopting the technology has the excellent comprehensive characteristics of high hardness, wear resistance, corrosion resistance, insulation and the like, and is widely applied to the fields of aviation, aerospace, navigation, machinery, electronics, decoration, traffic, textile and the like.
The micro-arc oxidation ceramic layer has insulating property, and many electronic products require corrosion resistance and wear resistance and also need to have conductive property in a local area, so that the local conductive area needs to be protected in the micro-arc oxidation processing process. In addition, because the micro-arc oxidation film layer mainly grows outwards, the assembly surfaces of shafts or holes with high assembly precision of certain sizes also need to be protected. Therefore, the local protection mode of micro-arc oxidation treatment is an urgent problem to be solved in the production process. The micro-arc oxidation process has the characteristics of high oxidation breakdown voltage (the voltage of the aluminum alloy can reach more than 650V), weak alkali or strong alkalinity of a solution, high temperature (more than about 2000 ℃) of partial discharge sparks and the like, so that the use requirement cannot be met by adopting the traditional anodic oxidation or electroplating protective coating, and the problems of long processing period, over-protection, high cost and the like exist when the tool is manufactured for protection.
Disclosure of Invention
The invention aims to provide the protective coating for micro-arc oxidation, which has the characteristics of low-temperature curing, good adhesion to valve metal and alloy thereof, acid resistance, alkali resistance and good protection in the micro-arc oxidation processing process.
The invention also aims to provide a preparation method for the protective coating, which has the characteristics of simple process, low cost and easy stripping of the micro-arc oxidation film layer.
The technical scheme adopted by the invention is that the protective coating for micro-arc oxidation comprises the following raw materials in percentage by mass:
44-48 percent of base resin, 6-8 percent of modified organic silicon resin, 6-8 percent of flame retardant, 2.7-4.0 percent of fumed silica, 0.3-0.6 percent of dimethyl silicone oil, 0.3-0.8 percent of defoaming agent, 1.5-2.5 percent of color paste and the balance of solvent.
The invention is also characterized in that:
the base resin consists of 6-15% of polyisobutylene, 15-20% of SBS resin and the balance of solvent; the solvent is dimethyl carbonate and butyl acetate.
The modified organic silicon resin comprises dihydroxy polydimethylsiloxane and a silane coupling agent; 95-98% of dihydroxy polydimethylsiloxane and 2-5% of silane coupling agent;
the viscosity of the dihydroxy polydimethylsiloxane is 3000-10000 mPa.S; the silane coupling agent is any one of an aminosilane coupling agent, a vinyl silane coupling agent, an acryloxy silane coupling agent and an epoxy silane coupling agent.
The flame retardant is any one or a mixture of any two of zinc borate, antimony trioxide, magnesium hydroxide and expandable graphite.
The particle size of the fumed silica is 25-50 nm.
The viscosity of the dimethyl silicone oil is 100-1000 mPa.S.
The defoaming agent is any one of BYK-085 and BYK-060N.
The color paste consists of kaolin, precipitated barium sulfate and titanium cobalt green; 63.60 to 73.42 percent of kaolin, 26.54 to 36.39 percent of precipitated barium sulfate and 0.01 to 0.04 percent of cobalt titanate green
The solvent is any one of tetrachloroethylene, xylene, dimethyl carbonate and butyl acetate.
The invention adopts another technical scheme that the preparation method of the protective coating for micro-arc oxidation is implemented according to the following steps:
step 1, preparing a base resin
Respectively pouring 6-15% of polyisobutylene and 15-20% of SBS resin in percentage by mass into respective reaction kettle, respectively adding dimethyl carbonate and butyl acetate for soaking, and stirring until the mixture is uniformly mixed to obtain base resin for later use;
step 2, preparing modified organic silicon resin
Mixing 95-98% of dihydroxy polydimethylsiloxane and 2-5% of silane coupling agent in percentage by mass at 60-120 ℃ under a vacuum condition of-0.09-0.1 MPa for 30-120 min, and cooling to room temperature to obtain modified organic silicon resin for later use;
step 3, adding 44-48% of base resin by mass into a movable tank, sequentially adding 6-8% of modified organic silicon resin by mass, 6-8% of flame retardant, 2.7-4.0% of fumed silica, 0.3-0.6% of dimethyl silicone oil, 0.3-0.8% of defoaming agent, 1.5-2.5% of color paste and the balance of solvent by mass, mixing, and uniformly stirring by using a high-speed stirrer to obtain a mixed material;
and 4, grinding the mixed material by using a sand mill, and testing the ground mixed material by using a scraper fineness meter until the fineness of the ground mixed material reaches below 30 mu m to obtain the protective coating for micro-arc oxidation.
The invention has the beneficial effects that:
(1) the protective coating for micro-arc oxidation has the characteristics of low-temperature curing, good adhesion to valve metal and alloy thereof, acid resistance and alkali resistance; by adding the improved organic silicon resin, the bonding strength of the peelable glue and the base materials of aluminum, magnesium, titanium and alloy thereof is effectively improved; the flame retardant is added, so that the carbonization phenomenon at the edge of the protective coating can be avoided; the addition of the fumed silica increases the sealing property and the seepage resistance of the product; the dimethyl silicone oil is added to ensure that the protective coating has good strippability; the protective coating can meet the requirements that when the thickness of the oxide layer is more than 50 mu m, the edges of the protective coating are neat and consistent, and the leakage phenomenon does not occur.
(2) The protective coating for micro-arc oxidation is prepared, the multifunctionality of the protective coating is expanded, the requirement of practical application can be met, and the protective coating has important significance for strengthening the practical application of the protective coating; the preparation method of the protective coating for micro-arc oxidation has the advantages of simple process and low cost.
Detailed Description
The present invention will be described in detail with reference to the following embodiments.
The invention relates to a protective coating for micro-arc oxidation, which comprises the following raw materials in percentage by mass:
44-48 percent of base resin, 6-8 percent of modified organic silicon resin, 6-8 percent of flame retardant, 2.7-4.0 percent of fumed silica, 0.3-0.6 percent of dimethyl silicone oil, 0.3-0.8 percent of defoaming agent, 1.5-2.5 percent of color paste and the balance of solvent.
The base resin consists of 6-15 percent of polyisobutylene and 15-20 percent of SBS resin by mass, and the balance of solvent; the solvent is dimethyl carbonate and butyl acetate.
The modified organic silicon resin comprises dihydroxy polydimethylsiloxane and a silane coupling agent; 95-98% of dihydroxy polydimethylsiloxane and 2-5% of silane coupling agent;
the viscosity of the dihydroxy polydimethylsiloxane is 3000-10000 mPa.S; the silane coupling agent is any one of an aminosilane coupling agent, a vinyl silane coupling agent, an acryloxy silane coupling agent and an epoxy silane coupling agent.
The flame retardant is any one or a mixture of any two of zinc borate, antimony trioxide, magnesium hydroxide and expandable graphite.
The particle size of the fumed silica is 25-50 nm.
The viscosity of the dimethyl silicone oil is 100-1000 mPa.S.
The defoaming agent is any one of BYK-085 and BYK-060N.
The color paste consists of kaolin, precipitated barium sulfate and titanium cobalt green; 63.60 to 73.42 percent of kaolin, 26.54 to 36.39 percent of precipitated barium sulfate and 0.01 to 0.04 percent of cobalt titanate green
The solvent is any one of tetrachloroethylene, xylene, dimethyl carbonate and butyl acetate.
The invention also relates to a preparation method of the protective coating for micro-arc oxidation, which is implemented according to the following steps:
step 1, preparing a base resin
Respectively pouring 6-15% of polyisobutylene and 15-20% of SBS resin in percentage by mass into respective reaction kettle, respectively adding dimethyl carbonate and butyl acetate for soaking, and stirring until the mixture is uniformly mixed to obtain base resin for later use;
step 2, preparing modified organic silicon resin
Mixing 95-98% of dihydroxy polydimethylsiloxane and 2-5% of silane coupling agent in percentage by mass at 60-120 ℃ under a vacuum condition of-0.09-0.1 MPa for 30-120 min, and cooling to room temperature to obtain modified organic silicon resin for later use;
step 3, adding 44-48% of base resin by mass into a movable tank, sequentially adding 6-8% of modified organic silicon resin by mass, 6-8% of flame retardant, 2.7-4.0% of fumed silica, 0.3-0.6% of dimethyl silicone oil, 0.3-0.8% of defoaming agent, 1.5-2.5% of color paste and the balance of solvent by mass, mixing, and uniformly stirring by using a high-speed stirrer to obtain a mixed material;
and 4, grinding the mixed material by using a sand mill, and testing the ground mixed material by using a scraper fineness meter until the fineness of the ground mixed material reaches below 30 mu m to obtain the protective coating for micro-arc oxidation.
Example 1
(1) Preparation of the base resin
Respectively pouring 6% of polyisobutylene and 15% of SBS resin in percentage by mass into respective reaction kettles, respectively adding 34% of dimethyl carbonate and 45% of butyl acetate for soaking, and stirring until the mixture is uniformly mixed to obtain base resin for later use;
(2) preparation of modified Silicone resins
Mixing 98% of dihydroxy polydimethylsiloxane and 2% of silane coupling agent by mass percent at 80 ℃ under a vacuum condition of-0.1 MPa for 60min, and cooling to room temperature to obtain modified organic silicon resin for later use;
wherein the viscosity of the dihydroxy polydimethylsiloxane is 5000 mPa.S; the silane coupling agent is an aminosilane coupling agent.
(3) Adding 44 mass percent of base resin into a movable tank, sequentially adding 8 mass percent of modified organic silicon resin, 8 mass percent of flame retardant, 2.7 mass percent of fumed silica, 0.6 mass percent of dimethyl silicone oil, 0.3 mass percent of defoaming agent, 1.5 mass percent of color paste and 34.9 mass percent of solvent for mixing, and uniformly stirring the mixture by adopting a high-speed stirrer to obtain a mixed material;
wherein the rotating speed of the high-speed stirrer is 2000 rpm; the flame retardant is zinc borate, the grain diameter of the fumed silica is 25nm, the viscosity of the dimethyl silicon oil is 200mPa.S, the defoaming agent is BYK-085, the color paste consists of 65 percent of kaolin, 34.98 percent of precipitated barium sulfate and 0.02 percent of titanium green cobalt, and the solvent is tetrachloroethylene.
(4) And (3) grinding the mixed material by using a sand mill, and testing the ground mixed material by using a scraper fineness meter until the fineness of the mixed material reaches below 30 mu m to obtain the protective coating for micro-arc oxidation.
Examples 2,
(1) Preparation of the base resin
Respectively pouring 8% of polyisobutylene and 20% of SBS resin in percentage by mass into respective reaction kettles, respectively adding 30% of dimethyl carbonate and 42% of butyl acetate for soaking, and stirring until the materials are uniformly mixed to obtain base resin for later use;
(2) preparation of modified Silicone resins
Mixing 95 mass percent of dihydroxy polydimethylsiloxane and 5 mass percent of silane coupling agent for 30min at 120 ℃ under vacuum condition of-0.09 MPa, and cooling to room temperature to obtain modified organic silicon resin for later use;
wherein the viscosity of the dihydroxy polydimethylsiloxane is 8000 mPa.S; the silane coupling agent is a vinyl silane coupling agent.
(3) Adding 48 mass percent of base resin into a movable tank, sequentially adding 6 mass percent of modified organic silicon resin, 7 mass percent of flame retardant, 3 mass percent of fumed silica, 0.3 mass percent of dimethyl silicone oil, 0.4 mass percent of defoaming agent, 2 mass percent of color paste and 33.3 mass percent of solvent for mixing, and uniformly stirring the mixture by adopting a high-speed stirrer to obtain a mixed material;
wherein the rotating speed of the high-speed stirrer is 2000 rpm; the flame retardant is magnesium hydroxide, the particle size of the fumed silica is 40nm, the viscosity of the dimethyl silicon oil is 500mPa.S, the defoaming agent is BYK-060N, the color paste consists of 70% of kaolin, 29.96% of precipitated barium sulfate and 0.04% of titanium green cobalt, and the solvent is dimethylbenzene.
(4) And (3) grinding the mixed material by using a sand mill, and testing the ground mixed material by using a scraper fineness meter until the fineness of the mixed material reaches below 30 mu m to obtain the protective coating for micro-arc oxidation.
Examples 3,
(1) Preparation of the base resin
Respectively pouring 7% of polyisobutylene and 18% of SBS resin in percentage by mass into respective reaction kettles, respectively adding 32% of dimethyl carbonate and 43% of butyl acetate for soaking, and stirring until the materials are uniformly mixed to obtain base resin for later use;
(2) preparation of modified Silicone resins
Mixing 96 percent of dihydroxy polydimethylsiloxane and 4 percent of silane coupling agent by mass percent at 100 ℃ under vacuum condition of-0.09 MPa for 40min, and cooling to room temperature to obtain modified organic silicon resin for later use;
wherein the viscosity of the dihydroxy polydimethylsiloxane is 10000 mPa.S; the silane coupling agent is propionyloxy siloxane.
(3) Adding 46 mass percent of base resin into a movable tank, sequentially adding 7 mass percent of modified organic silicon resin, 8 mass percent of flame retardant, 3.6 mass percent of fumed silica, 0.45 mass percent of dimethyl silicone oil, 0.5 mass percent of defoaming agent, 1.8 mass percent of color paste and 32.65 mass percent of solvent for mixing, and uniformly stirring the mixture by adopting a high-speed stirrer to obtain a mixed material;
wherein the rotating speed of the high-speed stirrer is 2000 rpm; the fire retardant is 60 percent of expandable graphite and 40 percent of antimony trioxide by mass, the grain diameter of the gas-phase silicon dioxide is 50nm, the viscosity of the dimethyl silicon oil is 1000mPa.S, the defoaming agent is BYK-085, the color paste consists of 66 percent of kaolin, 33.97 percent of precipitated barium sulfate and 0.03 percent of titanium green cobalt, and the solvent is dimethyl carbonate.
(4) And (3) grinding the mixed material by using a sand mill, and testing the ground mixed material by using a scraper fineness meter until the fineness of the mixed material reaches below 30 mu m to obtain the protective coating for micro-arc oxidation.
Example 4
(1) Preparation of the base resin
Respectively pouring 6% of polyisobutylene and 19% of SBS resin in percentage by mass into respective reaction kettles, respectively adding 31.5% of dimethyl carbonate and 43.5% of butyl acetate for soaking, and stirring until the mixture is uniformly mixed to obtain base resin for later use;
(2) preparation of modified Silicone resins
Mixing 95.5 mass percent of dihydroxy polydimethylsiloxane and 4.5 mass percent of silane coupling agent for 120min at 60 ℃ under the vacuum condition of-0.09 MPa, and cooling to room temperature to obtain modified organic silicon resin for later use;
wherein the viscosity of the dihydroxy polydimethylsiloxane is 7000 mPa.S; the silane coupling agent is an epoxy silane coupling agent.
(3) Adding 45 mass percent of base resin into a movable tank, sequentially adding 8 mass percent of modified organic silicon resin, 7 mass percent of flame retardant, 3 mass percent of fumed silica, 0.5 mass percent of dimethyl silicone oil, 0.8 mass percent of defoaming agent, 2.5 mass percent of color paste and 33.2 mass percent of solvent for mixing, and uniformly stirring the mixture by adopting a high-speed stirrer to obtain a mixed material;
wherein the rotating speed of the high-speed stirrer is 2000 rpm; the flame retardant is zinc borate, the grain diameter of the fumed silica is 30nm, the viscosity of the dimethyl silicon oil is 100mPa.S, the defoaming agent is BYK-060N, the color paste consists of 68% of kaolin, 31.95% of precipitated barium sulfate and 0.05% of cobalt titanate green, and the solvent is butyl acetate.
(4) And (3) grinding the mixed material by using a sand mill, and testing the ground mixed material by using a scraper fineness meter until the fineness of the mixed material reaches below 30 mu m to obtain the protective coating for micro-arc oxidation.
Example 5
(1) Preparation of the base resin
Respectively pouring 7.5% of polyisobutylene and 19.5% of SBS resin in percentage by mass into respective reaction kettles, respectively adding 33% of dimethyl carbonate and 40% of butyl acetate for soaking, and stirring until the mixture is uniformly mixed to obtain base resin for later use;
(2) preparation of modified Silicone resins
97.5 percent of dihydroxy polydimethylsiloxane and 2.5 percent of silane coupling agent in percentage by mass are mixed for 50min at 110 ℃ and under the vacuum condition of-0.1 MPa, and then the mixture is cooled to room temperature to obtain modified organic silicon resin for later use;
wherein the viscosity of the dihydroxy polydimethylsiloxane is 5000 mPa.S; the silane coupling agent is a vinyl silane coupling agent.
(3) Adding 47 mass percent of base resin into a movable tank, sequentially adding 7.5 mass percent of modified organic silicon resin, 6 mass percent of flame retardant, 4 mass percent of fumed silica, 0.35 mass percent of dimethyl silicone oil, 0.6 mass percent of defoaming agent, 2.2 mass percent of color paste and 32.35 mass percent of solvent for mixing, and uniformly stirring the mixture by adopting a high-speed stirrer to obtain a mixed material;
wherein the rotating speed of the high-speed stirrer is 2000 rpm; the flame retardant is zinc borate, the grain diameter of the fumed silica is 50nm, the viscosity of the dimethyl silicon oil is 500mPa.S, the defoaming agent is BYK-060N, the color paste consists of 65 percent of kaolin, 34.95 percent of precipitated barium sulfate and 0.05 percent of cobalt titanate green, and the solvent is dimethylbenzene.
(4) And (3) grinding the mixed material by using a sand mill, and testing the ground mixed material by using a scraper fineness meter until the fineness of the mixed material reaches below 30 mu m to obtain the protective coating for micro-arc oxidation.
The performance tests of the protective coatings for micro-arc oxidation prepared in examples 1 to 5 are shown in Table 1.
Table 1, Performance test of protective coating for micro-arc oxidation in examples 1 to 5
Figure BDA0002186461120000111
As can be seen from Table 1, aiming at the specific high voltage phenomenon in the micro-arc oxidation processing process, the siloxane resin introduced in the invention can effectively improve the pit breakdown capability of the protective coating; after a small amount of silane coupling agent is added to modify siloxane, the bonding strength between the protective coating and the matrix can be improved; adding a proper amount of dimethyl silicone oil to ensure that the protective coating is easily stripped from the matrix after the protection is finished; the addition of a proper amount of flame retardant can avoid the carbonization phenomenon of the edge caused by local sparks generated in the micro-arc oxidation process at the interface of the protective coating and the base material; the addition of the fumed silica increases the sealing property and the seepage resistance of the product; the defoaming agent is added, so that the condition that the product generates leakage protection in the middle, particularly the corner part, due to bubbles generated in the drying process of the protective coating can be avoided; the purpose of adding color paste is to distinguish the colors of the protective coating from the color of the substrate, so that the protective coating can be easily checked in actual operation and removed.

Claims (7)

1. The protective coating for micro-arc oxidation is characterized by comprising the following raw materials in percentage by mass:
44-48% of base resin, 6-8% of modified organic silicon resin, 6-8% of flame retardant, 2.7-4.0% of fumed silica, 0.3-0.6% of dimethyl silicone oil, 0.3-0.8% of defoaming agent, 1.5-2.5% of color paste and the balance of solvent;
the base resin consists of polyisobutylene, SBS resin, dimethyl carbonate and butyl acetate, the mass percent of the polyisobutylene is 6-15%, the mass percent of the SBS resin is 15-20%, and the balance is the dimethyl carbonate and the butyl acetate;
the viscosity of the dimethyl silicone oil is 100-1000 mPa.S;
the color paste consists of kaolin, precipitated barium sulfate and titanium cobalt green; the mass percent of the kaolin is 63.60-73.42%, the mass percent of the precipitated barium sulfate is 26.54-36.39%, and the mass percent of the cobalt titanate green is 0.01-0.04%;
the modified organic silicon resin comprises dihydroxy polydimethylsiloxane and a silane coupling agent.
2. The protective coating for micro-arc oxidation according to claim 1, wherein the dihydroxy polydimethylsiloxane is 95-98% by mass, and the silane coupling agent is 2-5% by mass;
the viscosity of the dihydroxy polydimethylsiloxane is 3000-10000 mPa.S; the silane coupling agent is any one of an aminosilane coupling agent, a vinyl silane coupling agent, an acryloxy silane coupling agent and an epoxy silane coupling agent.
3. The protective coating for micro-arc oxidation according to claim 1, wherein the flame retardant is any one or a mixture of any two of zinc borate, antimony trioxide, magnesium hydroxide and expandable graphite.
4. The protective coating for micro-arc oxidation according to claim 1, wherein the fumed silica has a particle size of 25 to 50 nm.
5. The protective coating for micro-arc oxidation according to claim 1, wherein the defoaming agent is any one of BYK-085 and BYK-060N.
6. The protective coating for micro-arc oxidation according to claim 1, wherein the solvent is any one of tetrachloroethylene, xylene, dimethyl carbonate and butyl acetate.
7. The preparation method of the protective coating for micro-arc oxidation according to any one of claims 1 to 6, which is implemented by the following steps:
step 1, preparing a base resin
Respectively pouring 6-15% of polyisobutylene and 15-20% of SBS resin in percentage by mass into respective reaction kettle, respectively adding dimethyl carbonate and butyl acetate for soaking, and stirring until the mixture is uniformly mixed to obtain base resin for later use;
step 2, preparing modified organic silicon resin
Mixing 95-98% of dihydroxy polydimethylsiloxane and 2-5% of silane coupling agent in percentage by mass at 60-120 ℃ under vacuum condition of-0.09-0.1 MPa for 30-120 min, and cooling to room temperature to obtain modified organic silicon resin for later use;
step 3, adding 44-48% of base resin by mass into a movable tank, sequentially adding 6-8% of modified organic silicon resin by mass, 6-8% of flame retardant by mass, 2.7-4.0% of fumed silica by mass, 0.3-0.6% of dimethyl silicone oil by mass, 0.3-0.8% of defoaming agent by mass, 1.5-2.5% of color paste by mass and the balance of solvent by mass, mixing, and uniformly stirring by using a high-speed stirrer to obtain a mixed material;
and 4, grinding the mixed material by using a sand mill, and testing the ground mixed material by using a scraper fineness meter until the fineness of the ground mixed material reaches below 30 mu m to obtain the protective coating for micro-arc oxidation.
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CN107079599A (en) * 2015-01-28 2017-08-18 惠普发展公司,有限责任合伙企业 Oxidized and coating article and preparation method thereof
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