CN103923560A - Waterborne electro-plating sealant and preparation method thereof - Google Patents
Waterborne electro-plating sealant and preparation method thereof Download PDFInfo
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Abstract
The invention relates to the technical field of polymer materials, and particularly discloses a polymer waterborne paint for surface hole-sealing protection of metal which is electro-plated with chromium and a preparation method of the polymer waterborne paint. An organo-silicon-modified electro-plating sealant is prepared from a film agent (organo-silicon-modified waterborne polyurethane), a filling material (silica sol), a defoamer and a leveling agent. The electro-plating sealant has strong adhesion to an electro-plated layer, and has good corrosion resistance, water resistance and wear resistance, wherein the specific indexes are as follows: the adhesion to the electro-plated layer is 0 level, the result of a salt-fog resistance experiment is more than or equal to 96 hours, the glossiness is more than 100, and the result of a water resistance experiment is more than or equal to 164 hours.
Description
Technical field
The present invention relates to technical field of polymer materials, be specifically related to high-molecular water paint of a kind of metal electric chromium plating rear surface sealing of hole protection and preparation method thereof.
Background technology
Metallic surface electrodeposited chromium is to strengthen corrosion resistance of metals and ornamental common method, but chromium coating inevitably can produce some holes and crackle in electroplating process, and its erosion resistance is reduced.A kind of effective ways that strengthen chromium coating corrosion-resistant are to stop up and seal micropore and the crack in coating at coating surface application one deck macromolecule resin, in order to the erosion of isolated foreign matter.
The conventional encapsulant of electroplating has solvent-borne type and the large class of water-based two.Solvent-borne type is due to the harm existing human and environment, gradually by watersoluble closed dose of replacement.Water-based is electroplated encapsulant, and to use at present the most general be water-borne acrylic resin, but that this class encapsulant exists is weather-proof, water tolerance is undesirable, reduces very soon with the prolongation in time of the plating piece etch resistant properties of its sealing.Waterborne organic silicon resin is the novel plating encapsulant of development in recent years, and it has and electrolytic coating strong adhesion, coating luminous, the advantage of water-tolerant.Pan Huiming etc. have reported a kind of waterborne organic silicon plating encapsulant of preparing with organosilane monomer, and CN102719121A has introduced low-temperature curing water-based metal anticorrosive coating prepared by a kind of hybrid inorganic-organic silane material.But more existing researchs point out, alone waterborne organic silicon resin is made encapsulant, and its salt spray resistance is unsatisfactory.
Summary of the invention
For the deficiencies in the prior art, the object of the present invention is to provide a kind of organic-silicon-modified aqueous polyurethane to electroplate encapsulant and preparation method thereof, make membrane-forming agent with organic-silicon-modified aqueous polyurethane, make filler with silicon sol, be aided with defoamer, flow agent is made organic-silicon-modified plating encapsulant, with electrolytic coating strong adhesion, there is good solidity to corrosion, water tolerance and wear resistance.Its specific targets are as follows: with 0 grade of electrolytic coating sticking power, and salt spray resistance experiment >=96 hours, glossiness is greater than 100, water-fast experiment >=164 hour.
Object of the present invention is mainly achieved through the following technical solutions:
A kind of water-based is electroplated encapsulant, and it is made up of the following component of weight part:
Organic-silicon-modified aqueous polyurethane 20-60 part, silicon sol 10-30 part, flow agent aqueous solution 1-5 part, defoamer aqueous solution 5-10 part are finally mended to 100 parts with deionized water;
Described organic-silicon-modified aqueous polyurethane is prepared as follows:
In four-hole boiling flask, drop into polyoxyethylene glycol, 2,2-dimethylol propionic acid, is warming up to 80 DEG C, vacuum hydro-extraction 2 hours; Be cooled to room temperature, add acetone, logical nitrogen, is stirred to 2,2-dimethylol propionic acid and dissolves completely, is warming up to 60 DEG C, slowly drips vulcabond, maintains 60 DEG C～65 DEG C reactions 4 hours, is warming up to 80 DEG C of reactions 0.5 hour; Then add 3-aminopropyl trimethoxysilane, react 1 hour, cool to 35 DEG C, add water and N methyldiethanol amine, speed with 1200r/min stirs 0.5 hour, then adds the ammoniacal liquor of 2M to be adjusted to pH=9～10, obtains transparent organic-silicon-modified aqueous polyurethane.
Described molecular weight polyethylene glycol is 400～2000;
Described vulcabond is any one in tolylene diisocyanate, isophorone diisocyanate, hexamethylene diisocyanate, Methylcyclohexyl diisocyanate.
Isocyanato in described vulcabond and hydroxyl (the hydroxyl sum in polyoxyethylene glycol and 2,2-dimethylol propionic acid) mol ratio (NCO/OH) is 1.05/1;
Described 2, the quality of 2-dimethylol propionic acid is 5.0% of polyoxyethylene glycol and vulcabond quality sum;
The mol ratio of described 3-aminopropyl trimethoxysilane and polyoxyethylene glycol is 1/5;
The mol ratio of described N methyldiethanol amine and polyoxyethylene glycol is 1/1;
The amount (volume) of described acetone is 1/1 (ml/g) with the ratio of the amount (quality) of polyoxyethylene glycol;
The quality adding water in described organic-silicon-modified aqueous polyurethane preparation process is 10 times of polyoxyethylene glycol quality;
Described silicon sol is prepared as follows:
The acetum 10ml of 1000ml water, 2M is added in 2000ml beaker, then slowly add 5g tetraethoxy, 20g3-aminopropyl triethoxysilane and 10g γ-(2,3-glycidoxy) propyl trimethoxy silicane, stir lower By Hydrolysis At Room Temperature 1 hour, then be adjusted to pH=8～9 with 2M ammoniacal liquor, be warming up to 100 DEG C, steam ethanol and obtain water white silicon sol.
The described flow agent aqueous solution is the silok-8255 water-based flow agent aqueous solution of 10% (mass percent).
The described defoamer aqueous solution is the SILCOLAPSE C546 waterborne organic silicon defoamer aqueous solution of 5% (mass percent).
Compared with prior art, advantage of the present invention and beneficial effect are:
1, have good weathering resistance and solidity to corrosion, coating is not easy to change, good decorative property.
2,, owing to having adopted organic-silicon-modified urethane and silicon sol compound system, the protective layer finally forming had both had good flexible, had again certain hardness; Aqueous high molecular coating hardness deficiency, the easy shortcoming scratching are overcome.
Embodiment
Applicant is described in detail product of the present invention and preparation method thereof in connection with specific embodiment below.
In following examples 1-6, the standard of the detection method of products obtained therefrom is as follows:
Electrolytic coating sticking power is pressed GB/T9286-1998 test;
GB/T10125-2012 test is pressed in salt spray resistance experiment;
Glossiness is pressed the method test in GB/T9754-2007;
Water-fast experiment is tested by the method 1 in GB/T1733-93.
Embodiment 1
A kind of water-based is electroplated encapsulant, is made up of organic-silicon-modified aqueous polyurethane, silicon sol, the flow agent aqueous solution, the defoamer aqueous solution and deionized water.
Wherein, the preparation method of organic-silicon-modified aqueous polyurethane is as follows:
In four-hole boiling flask, drop into 40.0g polyoxyethylene glycol (molecular weight 400), 3.1g2,2-dimethylol propionic acid, is warming up to 80 DEG C, vacuum hydro-extraction 2 hours; Be cooled to room temperature, add 40ml acetone, logical nitrogen, is stirred to 2,2-dimethylol propionic acid and dissolves completely, is warming up to 60 DEG C, slowly drips 21.9g tolylene diisocyanate, maintains 60 DEG C～65 DEG C reactions 4 hours, is then warming up to 80 DEG C of reactions 0.5 hour; Then add 3.58g3-aminopropyl trimethoxysilane, react 1 hour, cool to 35 DEG C, add 400ml water and 12.0g N methyldiethanol amine, speed with 1200r/min stirs 0.5 hour, adds the ammoniacal liquor of 2M to be adjusted to pH=9～10, obtains transparent organic-silicon-modified aqueous polyurethane.
Wherein, the preparation method of silicon sol is as follows:
The acetum 10ml of 1000ml water, 2M is added in 2000ml beaker, then slowly add 5g tetraethoxy, 20g3-aminopropyl triethoxysilane and 10g γ-(2,3-glycidoxy) propyl trimethoxy silicane, stir lower By Hydrolysis At Room Temperature 1 hour, with 2M ammoniacal liquor adjusting pH=8～9, be warming up to 100 DEG C, steam ethanol and obtain water white silicon sol.
Wherein, the flow agent aqueous solution is the silok-8255 water-based flow agent aqueous solution of 10% (mass percent).
The defoamer aqueous solution is the SILCOLAPSE C546 waterborne organic silicon defoamer aqueous solution of 5% (mass percent).
Above-mentioned organic-silicon-modified aqueous polyurethane 20g, silicon sol 30g, flow agent aqueous solution 1g, defoamer aqueous solution 5g and deionized water 44ml are uniformly mixed, obtain water-based and electroplate encapsulant.Experiment records this encapsulant and electrolytic coating sticking power is 0 grade, salt spray resistance experiment 96 hours, glossiness 100, water-fast experiment 172 hours.
Embodiment 2
A kind of water-based is electroplated encapsulant, is made up of organic-silicon-modified aqueous polyurethane, silicon sol, the flow agent aqueous solution, the defoamer aqueous solution and deionized water.
Wherein, the preparation method of organic-silicon-modified aqueous polyurethane is as follows:
In four-hole boiling flask, drop into 60.0g polyoxyethylene glycol (molecular weight 600), 4.6g2,2-dimethylol propionic acid, is warming up to 80 DEG C, vacuum hydro-extraction 2 hours; Be cooled to room temperature, add 60ml acetone, logical nitrogen, is stirred to 2,2-dimethylol propionic acid and dissolves completely, is warming up to 60 DEG C, slowly drips 31.3g isophorone diisocyanate, maintains 60 DEG C～65 DEG C reactions 4 hours, is warming up to 80 DEG C of reactions 0.5 hour; Then add 3.58g3-aminopropyl trimethoxysilane, react 1 hour, cool to 35 DEG C, add 600ml water and 12.0g N methyldiethanol amine, speed with 1200r/min stirs 0.5 hour, then add the ammoniacal liquor of 2M to regulate pH=9～10, obtain transparent organic-silicon-modified aqueous polyurethane.
Wherein, the preparation method of silicon sol is as follows:
The acetum 10ml of 1000ml water, 2M is added in 2000ml beaker, then slowly add 5g tetraethoxy, 20g3-aminopropyl triethoxysilane and 10g γ-(2,3-glycidoxy) propyl trimethoxy silicane, stir lower By Hydrolysis At Room Temperature 1 hour, then regulate pH=8～9 with 2M ammoniacal liquor, be warming up to 100 DEG C, steam ethanol and obtain water white silicon sol.
Wherein, the flow agent aqueous solution is the silok-8255 water-based flow agent aqueous solution of 10% (mass percent).
The defoamer aqueous solution is the SILCOLAPSE C546 waterborne organic silicon defoamer aqueous solution of 5% (mass percent).
Above-mentioned organic-silicon-modified aqueous polyurethane 30g, silicon sol 20g, defoamer aqueous solution 7g, flow agent aqueous solution 3g and deionized water 40ml are uniformly mixed, obtain water-based and electroplate encapsulant.Experiment records this encapsulant and electrolytic coating sticking power is 0 grade, salt spray resistance experiment 126 hours, glossiness 105, water-fast experiment 182 hours.
Embodiment 3
A kind of water-based is electroplated encapsulant, is made up of organic-silicon-modified aqueous polyurethane, silicon sol, the flow agent aqueous solution, the defoamer aqueous solution and deionized water.
Wherein, the preparation method of organic-silicon-modified aqueous polyurethane is as follows:
In four-hole boiling flask, drop into 60.0g polyoxyethylene glycol (molecular weight 600), 4.2g2,2-dimethylol propionic acid, is warming up to 80 DEG C, vacuum hydro-extraction 2 hours; Be cooled to room temperature, add 60ml acetone, logical nitrogen, is stirred to 2,2-dimethylol propionic acid and dissolves completely, is warming up to 60 DEG C, slowly drips 23.1g1, and hexamethylene-diisocyanate maintains 60 DEG C～65 DEG C reactions 4 hours, is warming up to 80 DEG C of reactions 0.5 hour.Then add 3.58g3-aminopropyl trimethoxysilane, react 1 hour, cool to 35 DEG C, add 600ml water and 12.0g N methyldiethanol amine, speed with 1200r/min stirs 0.5 hour, then add the ammoniacal liquor of 2M to regulate pH=9～10, obtain transparent organic-silicon-modified aqueous polyurethane.
Wherein, the preparation method of silicon sol is as follows:
The acetum 10ml of 1000ml water, 2M is added in 2000ml beaker, then slowly add 5g tetraethoxy, 20g3-aminopropyl triethoxysilane and 10g γ-(2,3-glycidoxy) propyl trimethoxy silicane, stir lower By Hydrolysis At Room Temperature 1 hour, then regulate pH=8～9 with 2M ammoniacal liquor, be warming up to 100 DEG C, steam ethanol and obtain water white silicon sol.
Wherein, the flow agent aqueous solution is the silok-8255 water-based flow agent aqueous solution of 10% (mass percent).
The defoamer aqueous solution is the SILCOLAPSE C546 waterborne organic silicon defoamer aqueous solution of 5% (mass percent).
Above-mentioned organic-silicon-modified aqueous polyurethane 35g, silicon sol 15g, defoamer aqueous solution 7g, flow agent aqueous solution 4g and deionized water 39ml are uniformly mixed, obtain water-based and electroplate encapsulant.Experiment records this encapsulant and electrolytic coating sticking power is 0 grade, salt spray resistance experiment 134 hours, glossiness 105, water-fast experiment 176 hours.
Embodiment 4
A kind of water-based is electroplated encapsulant, is made up of organic-silicon-modified aqueous polyurethane, silicon sol, the flow agent aqueous solution, the defoamer aqueous solution and deionized water.
Wherein, the preparation method of organic-silicon-modified aqueous polyurethane is as follows:
In four-hole boiling flask, drop into 100.0g polyoxyethylene glycol (molecular weight 1000), 6.8g2,2-dimethylol propionic acid, is warming up to 80 DEG C, vacuum hydro-extraction 2 hours; Be cooled to room temperature, add the acetone of 100ml, logical nitrogen, is stirred to 2,2-dimethylol propionic acid and dissolves completely, is warming up to 60 DEG C, slowly drips 35.2g isophorone diisocyanate, maintains 60 DEG C～65 DEG C reactions 4 hours, is warming up to 80 DEG C of reactions 0.5 hour; Then add 3.58g3-aminopropyl trimethoxysilane, react 1 hour, cool to 35 DEG C, add 1000ml water and 12.0g N methyldiethanol amine, speed with 1200r/min stirs 0.5 hour, then add the ammoniacal liquor of 2M to regulate pH=9～10, obtain transparent organic-silicon-modified aqueous polyurethane.
Wherein, the preparation method of silicon sol is as follows:
The acetum 10ml of 1000ml water, 2M is added in 2000ml beaker, then slowly add 5g tetraethoxy, 20g3-aminopropyl triethoxysilane and 10g γ-(2,3-glycidoxy) propyl trimethoxy silicane, stir lower By Hydrolysis At Room Temperature 1 hour, then regulate pH=8～9 with 2M ammoniacal liquor, be warming up to 100 DEG C, steam ethanol and obtain water white silicon sol.
Wherein, the flow agent aqueous solution is the silok-8255 water-based flow agent aqueous solution of 10% (mass percent).
The defoamer aqueous solution is the SILCOLAPSE C546 waterborne organic silicon defoamer aqueous solution of 5% (mass percent).
Above-mentioned organic-silicon-modified aqueous polyurethane 40g, silicon sol 20g, defoamer aqueous solution 8g, flow agent aqueous solution 4g and deionized water 28ml are uniformly mixed, obtain water-based and electroplate encapsulant.Experiment records this encapsulant and electrolytic coating sticking power is 0 grade, salt spray resistance experiment 178 hours, glossiness 110, water-fast experiment 168 hours.
Embodiment 5
A kind of water-based is electroplated encapsulant, is made up of organic-silicon-modified aqueous polyurethane, silicon sol, the flow agent aqueous solution, the defoamer aqueous solution and deionized water.
Wherein, the preparation method of organic-silicon-modified aqueous polyurethane is as follows:
In four-hole boiling flask, drop into 200.0g polyoxyethylene glycol (molecular weight 2000), 11.77g2,2-dimethylol propionic acid, is warming up to 80 DEG C, vacuum hydro-extraction 2 hours; Be cooled to room temperature, add 200ml acetone, logical nitrogen, is stirred to 2,2-dimethylol propionic acid and dissolves completely, is warming up to 60 DEG C, slowly drips 35.49g Methylcyclohexyl diisocyanate, maintains 60 DEG C～65 DEG C reactions 4 hours, is warming up to 80 DEG C of reactions 0.5 hour.Then add 3.58g3-aminopropyl trimethoxysilane, react 1 hour, cool to 35 DEG C, add 2000ml water and 12.0g N methyldiethanol amine, speed with 1200r/min stirs 0.5 hour, then add the ammoniacal liquor of 2M to regulate pH=9～10, obtain the translucent organic-silicon-modified aqueous polyurethane of oyster white.
Wherein, the preparation method of silicon sol is as follows:
The acetum 10ml of 1000ml water, 2M is added in 2000ml beaker, then slowly add 5g tetraethoxy, 20g3-aminopropyl triethoxysilane and 10g γ-(2,3-glycidoxy) propyl trimethoxy silicane, stir lower By Hydrolysis At Room Temperature 1 hour, then regulate pH=8～9 with 2M ammoniacal liquor, be warming up to 100 DEG C, steam ethanol and obtain water white silicon sol.
Wherein, the flow agent aqueous solution is the silok-8255 water-based flow agent aqueous solution of 10% (mass percent).
The defoamer aqueous solution is the SILCOLAPSE C546 waterborne organic silicon defoamer aqueous solution of 5% (mass percent).
Above-mentioned organic-silicon-modified aqueous polyurethane 50g, silicon sol 15g, defoamer aqueous solution 8g, flow agent aqueous solution 5g and deionized water 22ml are uniformly mixed, obtain water-based and electroplate encapsulant.Experiment records this encapsulant and electrolytic coating sticking power is 0 grade, salt spray resistance experiment 96 hours, glossiness 105, water-fast experiment 164 hours.
Embodiment 6
A kind of water-based is electroplated encapsulant, is made up of organic-silicon-modified aqueous polyurethane, silicon sol, the flow agent aqueous solution, the defoamer aqueous solution and deionized water.
Wherein, the preparation method of organic-silicon-modified aqueous polyurethane is as follows:
In four-hole boiling flask, drop into 40.0g polyoxyethylene glycol (molecular weight 400), 3.47g2,2-dimethylol propionic acid, is warming up to 80 DEG C, vacuum hydro-extraction 2 hours; Be cooled to room temperature, add 40ml acetone, logical nitrogen, is stirred to 2,2-dimethylol propionic acid and dissolves completely, is warming up to 60 DEG C, slowly drips 29.4g isophorone diisocyanate, maintains 60 DEG C～65 DEG C reactions 4 hours, is warming up to 80 DEG C of reactions 0.5 hour; Then add 3.58g3-aminopropyl trimethoxysilane, react 1 hour, cool to 35 DEG C, add 400ml water and 12.0g N methyldiethanol amine, speed with 1200r/min stirs 0.5 hour, then add the ammoniacal liquor of 2M to regulate pH=9～10, obtain transparent organic-silicon-modified aqueous polyurethane.
Wherein, the preparation method of silicon sol is as follows:
The acetum 10ml of 1000ml water, 2M is added in 2000ml beaker, then slowly add 5g tetraethoxy, 20g3-aminopropyl triethoxysilane and 10g γ-(2,3-glycidoxy) propyl trimethoxy silicane, stir lower By Hydrolysis At Room Temperature 1 hour, then regulate pH=8～9 with 2M ammoniacal liquor, be warming up to 100 DEG C, steam ethanol and obtain water white silicon sol.
Wherein, the flow agent aqueous solution is the silok-8255 water-based flow agent aqueous solution of 10% (mass percent).
The defoamer aqueous solution is the SILCOLAPSE C546 waterborne organic silicon defoamer aqueous solution of 5% (mass percent).
Above-mentioned organic-silicon-modified aqueous polyurethane 60g, silicon sol 10g, defoamer aqueous solution 10g, flow agent aqueous solution 5g and deionized water 15ml are uniformly mixed, obtain water-based and electroplate encapsulant.Experiment records this encapsulant and electrolytic coating sticking power is 0 grade, salt spray resistance experiment 176 hours, glossiness 105, water-fast experiment 198 hours.
Claims (7)
1. water-based is electroplated an encapsulant, and it is made up of the following component of weight part:
Organic-silicon-modified aqueous polyurethane 20-60 part, silicon sol 10-30 part, flow agent aqueous solution 1-5 part, defoamer aqueous solution 5-10 part, deionized water is mended to 100 parts;
Described organic-silicon-modified aqueous polyurethane is prepared as follows:
Drop into polyoxyethylene glycol, 2,2-dimethylol propionic acid, is warming up to 80 DEG C, vacuum hydro-extraction 2 hours; Be cooled to room temperature, add acetone, logical nitrogen, is stirred to 2,2-dimethylol propionic acid and dissolves completely, is warming up to 60 DEG C, drips vulcabond, maintains 60 DEG C～65 DEG C reactions 4 hours, is warming up to 80 DEG C of reactions 0.5 hour; Then add 3-aminopropyl trimethoxysilane, react 1 hour, cool to 35 DEG C, add water and N methyldiethanol amine, speed with 1200r/min stirs 0.5 hour, then adds the ammoniacal liquor of 2M to be adjusted to pH=9～10, obtains transparent organic-silicon-modified aqueous polyurethane;
Described molecular weight polyethylene glycol is 400～2000;
Described vulcabond is any one in tolylene diisocyanate, isophorone diisocyanate, hexamethylene diisocyanate, Methylcyclohexyl diisocyanate;
Described silicon sol is prepared as follows:
The acetum 10ml of 1000ml water, 2M is added in 2000ml beaker, then add 5g tetraethoxy, 20g 3-aminopropyl triethoxysilane and 10g γ-(2,3-glycidoxy) propyl trimethoxy silicane, stir lower By Hydrolysis At Room Temperature 1 hour, then be adjusted to pH=8～9 with 2M ammoniacal liquor, be warming up to 100 DEG C, steam ethanol and obtain water white silicon sol;
The silok-8255 water-based flow agent aqueous solution that the described flow agent aqueous solution is 10%;
The SILCOLAPSE C546 waterborne organic silicon defoamer aqueous solution that the described defoamer aqueous solution is 5%.
2. water-based according to claim 1 is electroplated encapsulant, it is characterized in that: described vulcabond
In isocyanato and the mol ratio of hydroxyl be 1.05/1;
Described hydroxyl is the hydroxyl sum in polyoxyethylene glycol and 2,2-dimethylol propionic acid.
3. water-based according to claim 1 is electroplated encapsulant, it is characterized in that: described 2, the quality of 2-dimethylol propionic acid is 5.0% of polyoxyethylene glycol and vulcabond quality sum.
4. water-based according to claim 1 is electroplated encapsulant, it is characterized in that: the mol ratio of described 3-aminopropyl trimethoxysilane and polyoxyethylene glycol is 1/5.
5. water-based according to claim 1 is electroplated encapsulant, it is characterized in that: the mol ratio of described N methyldiethanol amine and polyoxyethylene glycol is 1/1.
6. water-based according to claim 1 is electroplated encapsulant, it is characterized in that: the usage ratio of described acetone and polyoxyethylene glycol is 1mL/1g.
7. water-based according to claim 1 is electroplated encapsulant, it is characterized in that: the quality adding water in described organic-silicon-modified aqueous polyurethane preparation process is 10 times of polyoxyethylene glycol quality.
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