CN106634516B - High-corrosion-resistance water-based electroplating sealing agent and preparation method thereof - Google Patents
High-corrosion-resistance water-based electroplating sealing agent and preparation method thereof Download PDFInfo
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- 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
- C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
- C09D175/04—Polyurethanes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/08—Processes
- C08G18/10—Prepolymer processes involving reaction of isocyanates or isothiocyanates with compounds having active hydrogen in a first reaction step
- C08G18/12—Prepolymer processes involving reaction of isocyanates or isothiocyanates with compounds having active hydrogen in a first reaction step using two or more compounds having active hydrogen in the first polymerisation step
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/30—Low-molecular-weight compounds
- C08G18/34—Carboxylic acids; Esters thereof with monohydroxyl compounds
- C08G18/348—Hydroxycarboxylic acids
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/42—Polycondensates having carboxylic or carbonic ester groups in the main chain
- C08G18/44—Polycarbonates
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/65—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
- C08G18/66—Compounds of groups C08G18/42, C08G18/48, or C08G18/52
- C08G18/6633—Compounds of group C08G18/42
- C08G18/6659—Compounds of group C08G18/42 with compounds of group C08G18/34
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/54—Silicon-containing compounds
- C08K5/541—Silicon-containing compounds containing oxygen
- C08K5/5435—Silicon-containing compounds containing oxygen containing oxygen in a ring
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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
- 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
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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
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/48—After-treatment of electroplated surfaces
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Abstract
The invention relates to the technical field of fine polymers, in particular to a high-corrosion-resistance water-based electroplating sealant and a preparation method thereof. According to the invention, the carbon dioxide-based copolymer polyol is used as the electroplating sealant for the first time, and the corrosion resistance of the plating layer is greatly improved by utilizing the excellent oxygen barrier property of the carbon dioxide-based copolymer polyol; the sealant with high hardness and high wear resistance is obtained by organic-inorganic compounding. Meanwhile, the carbon dioxide copolymer polyol is used for preparation, so that the defects that the water-based coating prepared from polyether polyol is low in hardness and the water-based coating prepared from polyester polyol is easy to hydrolyze and fall off are overcome, and the electroplating sealant with hardness and toughness combined is formed.
Description
Technical Field
The invention relates to the technical field of fine polymers, in particular to a high-corrosion-resistance water-based electroplating sealant and a preparation method thereof.
Background
In the use process of the metal material, corrosion can be generated under different conditions, the plasticity and the toughness of the metal can be obviously reduced after the metal is corroded, and the service life of the metal is greatly shortened. In order to improve the corrosion resistance, the surface of steel and iron metal is often galvanized and passivated to improve the corrosion resistance, and meanwhile, the appearance of the product can be improved to provide certain decoration. The traditional zinc and zinc alloy passivation process generally adopts chromate passivation, has low cost, simple use and good corrosion resistance, and is widely applied in the fields of aviation, electronics and other industries. Chromium in the chromate passive film mainly exists in a hexavalent form and a trivalent form, the trivalent chromium is used as a framework of the passive film, and the hexavalent chromium can passivate a plating layer on the exposed part of the passive film again, so that the hexavalent chromium can further inhibit corrosion. However, hexavalent chromium has a certain carcinogenicity, and when used in a large amount, the hexavalent chromium seriously pollutes the environment and affects the health of human beings, and the european union has formally implemented the RoHS instruction in 1/7 2006 to limit the use of hexavalent chromium. Trivalent chromium has characteristics very similar to hexavalent chromium in many respects, while it has the advantage of low toxicity.
In order to enhance the corrosion resistance of the chromium plating layer, a sealing agent is mostly adopted to coat a layer of high molecular resin on the surface of the plating layer to block and seal micropores and cracks in the plating layer so as to isolate the corrosion of foreign substances.
Acrylic resin is added into passivation solution of the azolla (study on passivation process of trivalent chromium of a zinc coating, corrosion and protection, 2007, 28(1), 13-16, 19) and the like, and it is found that cracks on the surface of a trivalent chromium passivation film are completely covered by the acrylic resin, and the density of the film is improved. The trivalent chromium and the acrylic resin are adopted for passivation, so that the time of white rust on a zinc coating can be delayed, and the corrosion resistance is obviously improved compared with a film layer which is under the same condition and is not added with the acrylic resin. The acrylic resin has poor water resistance and causes corrosion after long-term water immersion. Chinese patent CN102719121A describes a low-temperature curing water-based metal anticorrosive paint prepared from organic-inorganic hybrid silane materials. However, some studies have shown that the salt spray resistance of the sealant is not satisfactory when a water-based silicone resin is used alone. The Chinese patent CN103923560B uses organic silicon modified polyethylene glycol type polyurethane aqueous solution to prepare a water-soluble sealant, and the salt mist resistance is greatly improved. However, because polyethylene glycol is a water-soluble polymer, the product is easy to absorb moisture and generate corrosion in the using process, and meanwhile, the hardness of the polyurethane layer is low, and the long-term wear resistance is poor.
Disclosure of Invention
The first purpose of the invention is to provide a water-based electroplating sealing agent with high corrosion resistance against the defects of the prior art.
The invention also aims to provide a preparation method of the water-based electroplating sealing agent with high corrosion resistance.
In order to achieve the above purpose, the present invention provides the following technical solutions:
an aqueous electroplating sealing agent with high corrosion resistance comprises the following components in parts by weight:
preferably, the water-based electroplating sealing agent with high corrosion resistance comprises the following components in parts by weight:
preferably, the carbon dioxide-based copolymer polyol is diol synthesized by copolymerizing carbon dioxide serving as a starting material and propylene oxide under the action of an initiator and a catalyst, and has the hydroxyl functionality of 2 and the molecular weight of 2000-4000.
Further preferably, the molecular weight of the carbon dioxide-based copolymer polyol is 3000-4000.
Preferably, the aliphatic diisocyanate is any one or a mixture of isophorone diisocyanate, hexamethylene diisocyanate and hydrogenated diphenylmethane diisocyanate.
Preferably, the hydrophilic chain extender is any one or a mixture of more of ethylenediamine ethanesulfonic acid sodium salt, 1, 4-butanediol-2-sulfonic acid sodium salt, dimethylolbutyric acid and dimethylolpropionic acid.
Preferably, the catalyst is any one or a mixture of stannous octoate and dibutyltin dilaurate.
Preferably, the neutralizing agent is one or a mixture of more of triethylamine, tripropylamine, tributylamine, sodium hydroxide and ammonia water.
Preferably, the chain extender is any one or a mixture of ethylene diamine, trimethylhexamethylene diamine, tetraethylenepentamine and diethylenetriamine.
Preferably, the aqueous leveling agent is a silok-8255 aqueous leveling agent aqueous solution with the mass percent of 5%.
Preferably, the aqueous defoaming agent is a 5% by mass aqueous silcolapse C546 aqueous silicone defoaming agent solution.
A preparation method of an aqueous electroplating sealant comprises the following steps:
taking 60 parts of carbon dioxide-based copolymer polyol, 20-60 parts of aliphatic diisocyanate, 3-6 parts of hydrophilic chain extender and 0.05-0.5 part of catalyst, heating to 80-95 ℃, reacting for 3-5h, cooling to about 35 ℃, adding a neutralizer for neutralization until the pH value reaches 7, adding KH-5600.5-2 parts, stirring for reaction for 1-2h, adding 150-200 parts of deionized water for emulsification, adding 0.5-2 parts of chain extender for chain extension, then adding 3-5 parts of hexyl orthosilicate, adding ammonia water for adjusting the pH value to 8-10, stirring for 1-2h, adding 1-5 parts of aqueous flatting agent and 1-5 parts of aqueous defoaming agent, and obtaining the aqueous electroplating sealant.
Preferably, the neutralizing agent is one or a mixture of more of triethylamine, tripropylamine, tributylamine, sodium hydroxide and ammonia water.
Compared with the prior art, the invention has the beneficial effects that:
the invention provides a high-corrosion-resistance water-based electroplating sealant and a preparation method thereof. According to the invention, the carbon dioxide-based copolymer polyol is used as the electroplating sealant for the first time, and the corrosion resistance of the plating layer is greatly improved by utilizing the excellent oxygen barrier property of the carbon dioxide-based copolymer polyol; the sealant with high hardness and high wear resistance is obtained by organic-inorganic compounding. Meanwhile, the carbon dioxide-based copolymer polyol is used for preparation, so that the defects that the water-based coating prepared from polyether polyol is low in hardness and the water-based coating prepared from polyester polyol is easy to hydrolyze and fall off are overcome, and the electroplating sealant with hardness and toughness combined is formed.
Detailed Description
The present invention will be described in further detail with reference to the following examples, which are not intended to limit the scope of the invention.
In examples 1 to 5 below, the test method for the obtained products was as follows, the plating adhesion was measured in accordance with GB/T9286-1998; the salt spray resistance test is tested according to GB/T10125-2012; water resistance tests were tested according to method 1 of GB/T1733-93.
Example 1.
Taking 60 parts of carbon dioxide-based copolymer polyol, 25 parts of isophorone diisocyanate, 4.7 parts of hydrophilic chain extender dimethylolpropionic acid and 0.1 part of stannous octoate, heating to 80 ℃, reacting for 3 hours, cooling to about 35 ℃, adding triethylamine to neutralize to a pH value of about 7, adding KH-5601 parts, stirring to react for 1-2 hours, adding 200 parts of deionized water to emulsify, adding 1 part of ethylenediamine to extend the chain of the chain extender, then adding 3 parts of hexyl orthosilicate, adding ammonia water to adjust the pH value to 8-10, stirring for 2 hours, adding 5 parts of silok-8255 aqueous leveling agent aqueous solution with the mass percentage of 5% and 5 parts of aqueous defoaming agent to obtain the aqueous electroplating sealant.
The adhesion force of the sealant and an electroplated layer is 0 grade through experimental tests, the salt spray resistance experiment is carried out for 144h, the water resistance experiment is carried out for 168h, and the hot water resistance experiment is carried out for 5 h.
Example 2.
Taking 60 parts of carbon dioxide-based copolymer polyol, 20 parts of diisocyanate, 3 parts of hydrophilic chain extender dimethylolpropionic acid and 0.2 part of catalyst, heating to 80 ℃, reacting for 5 hours, cooling to about 35 ℃, adding a neutralizing agent for neutralizing to about pH 7, adding KH-5600.5 parts, stirring for reacting for 1 hour, adding 150 parts of deionized water for emulsification, adding 0.5 part of diethylenetriamine, then chain extending the chain extender, then adding 3 parts of hexyl orthosilicate, adding ammonia water for regulating the pH to 10, stirring for 1 hour, adding 1 part of aqueous flatting agent and 1 part of aqueous defoaming agent, and obtaining the aqueous electroplating sealant.
The adhesion force of the sealant and an electroplated layer is 0 grade through experimental tests, and the salt spray resistance experiment lasts for 168 hours, the water resistance experiment lasts for 240 hours, and the hot water resistance experiment lasts for 8 hours.
Example 3.
Taking 60 parts of carbon dioxide-based copolymer polyol, 60 parts of hydrogenated diphenylmethane diisocyanate, 6 parts of hydrophilic chain extender dimethylolbutyric acid and 0.5 part of stannous octoate, heating to 80 ℃, reacting for 3 hours, cooling to about 35 ℃, adding triethylamine to neutralize to about pH 7, adding KH-5602 parts, stirring to react for 2 hours, adding 200 parts of deionized water to emulsify, adding 2 parts of chain extender to chain extend, then adding 5 parts of hexyl orthosilicate, adding ammonia water to adjust the pH to 10, stirring for 2 hours, adding 5 parts of silok-8255 aqueous flatting agent aqueous solution with the mass percent of 5% and 5 parts of aqueous defoamer to obtain the aqueous electroplating sealant.
The adhesion force of the sealant and an electroplated layer is 0 grade through experimental tests, the salt spray resistance experiment lasts for 96 hours, the water resistance experiment lasts for 168 hours, and the hot water resistance experiment lasts for 5 hours.
Example 4.
Taking 60 parts of carbon dioxide-based copolymer polyol, 20 parts of isophorone diisocyanate, 5 parts of hexamethylene diisocyanate, 4.7 parts of hydrophilic chain extender dimethylolpropionic acid and 0.2 part of stannous octoate, heating to 90 ℃, reacting for 4 hours, cooling to about 35 ℃, adding ammonia water to neutralize to about 7 pH value, adding KH-5601 parts, stirring to react for 2 hours, adding 180 parts of deionized water to emulsify, adding 1.5 parts of chain extender for chain extension, then adding 4 parts of hexyl orthosilicate, adding ammonia water to adjust the pH value to 8, stirring for 2 hours, adding 5 parts of silok-8255 aqueous leveling agent aqueous solution with the mass percentage of 5% and 5 parts of aqueous defoaming agent to obtain the aqueous electroplating sealant.
The adhesion force of the sealant and an electroplated layer is 0 grade through experimental tests, and the salt spray resistance experiment is 144h, the water resistance experiment is 196h, and the hot water resistance experiment is 6 h.
Example 5.
Taking 60 parts of carbon dioxide-based copolymer polyol, 25 parts of isophorone diisocyanate, 4.7 parts of hydrophilic chain extender dimethylolpropionic acid and 0.1 part of stannous octoate, heating to 90 ℃, reacting for 4 hours, cooling to about 35 ℃, adding triethylamine to neutralize to a pH value of about 7, adding KH-5601.5 parts, stirring to react for 1-2 hours, adding 150 parts of deionized water to emulsify, adding 1 part of chain extender to chain extend, then adding 3.5 parts of hexyl orthosilicate, adding ammonia water to adjust the pH value to 8, stirring for 2 hours, adding 5 parts of silok-8255 aqueous leveling agent aqueous solution with the mass percentage of 5% and 5 parts of aqueous defoaming agent to obtain the aqueous electroplating sealant.
The adhesion force of the sealant and an electroplated layer is 0 grade through experimental tests, the salt spray resistance experiment is carried out for 144h, the water resistance experiment is carried out for 168h, and the hot water resistance experiment is carried out for 5 h.
According to the invention, the carbon dioxide-based copolymer polyol is used as the electroplating sealant for the first time, and the corrosion resistance of the plating layer is greatly improved by utilizing the excellent oxygen barrier property of the carbon dioxide-based copolymer polyol; the sealant with high hardness and high wear resistance is obtained by organic-inorganic compounding. Meanwhile, the carbon dioxide-based copolymer polyol is used for preparation, so that the defects that the water-based coating prepared from polyether polyol is low in hardness and the water-based coating prepared from polyester polyol is easy to hydrolyze and fall off are overcome, and the electroplating sealant with hardness and toughness combined is formed.
The above-mentioned embodiments are only preferred embodiments of the present invention, and the scope of the present invention is not limited thereto, and therefore, the scope of the present invention is covered by the claims equivalent to the modifications of the present invention.
Claims (9)
1. The water-based electroplating sealing agent with high corrosion resistance is characterized by comprising the following components in parts by weight:
taking 60 parts of carbon dioxide-based copolymer polyol, 20-60 parts of aliphatic diisocyanate, 3-6 parts of hydrophilic chain extender and 0.05-0.5 part of catalyst, heating to 80-95 ℃, reacting for 3-5h, cooling to 35 ℃, adding a neutralizer for neutralization until the pH value reaches 7, adding KH-5600.5-2 parts, stirring for reaction for 1-2h, adding 150-200 parts of deionized water for emulsification, adding 0.5-2 parts of chain extender for chain extension, then adding 3-5 parts of hexyl orthosilicate, adding ammonia water for adjusting the pH value to 8-10, stirring for 1-2h, adding 1-5 parts of aqueous flatting agent and 1-5 parts of aqueous defoaming agent, and obtaining the aqueous electroplating sealant.
2. The aqueous electroplating sealant with high corrosion resistance according to claim 1, which comprises the following components in parts by weight:
3. the aqueous electroplating sealing agent with high corrosion resistance as defined in claim 1 or 2, wherein the carbon dioxide-based copolymer polyol is a diol copolymerized with propylene oxide under the action of an initiator and a catalyst by using carbon dioxide as a starting material, and has a hydroxyl functionality of 2 and a molecular weight of 2000-4000.
4. The aqueous electroplating sealant with high corrosion resistance according to claim 1 or 2, wherein the aliphatic diisocyanate is any one or a mixture of isophorone diisocyanate, hexamethylene diisocyanate and hydrogenated diphenylmethane diisocyanate.
5. The aqueous electroplating sealing agent with high corrosion resistance according to claim 1 or 2, wherein the hydrophilic chain extender is any one or a mixture of ethylene diamine ethyl sodium sulfonate, 1, 4-butanediol-2-sodium sulfonate, dimethylol butyric acid and dimethylol propionic acid.
6. The aqueous electroplating sealant with high corrosion resistance according to claim 1 or 2, wherein the catalyst is any one or a mixture of stannous octoate and dibutyltin dilaurate.
7. The aqueous electroplating sealing agent with high corrosion resistance according to claim 1 or 2, wherein the chain extender is any one or a mixture of ethylene diamine, trimethyl hexamethylene diamine, tetraethylene pentamine and diethylenetriamine.
8. The aqueous electroplating sealant with high corrosion resistance according to claim 1 or 2, wherein the aqueous leveling agent is a 5% by mass silok-8255 aqueous leveling agent aqueous solution, and the aqueous defoaming agent is a 5% by mass silcolapse C546 aqueous silicone defoaming agent aqueous solution.
9. The aqueous electroplating sealing agent with high corrosion resistance according to claim 1, wherein the neutralizing agent is any one or a mixture of triethylamine, tripropylamine, tributylamine, sodium hydroxide and ammonia water.
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| EP3283547B1 (en) * | 2015-04-13 | 2021-05-19 | Repsol, S.A. | New formulations for polyurethane applications |
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