CN105482585A - Preparation method of nano silicon dioxide-acrylic resin composite coating - Google Patents
Preparation method of nano silicon dioxide-acrylic resin composite coating Download PDFInfo
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- CN105482585A CN105482585A CN201510992028.2A CN201510992028A CN105482585A CN 105482585 A CN105482585 A CN 105482585A CN 201510992028 A CN201510992028 A CN 201510992028A CN 105482585 A CN105482585 A CN 105482585A
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- C—CHEMISTRY; METALLURGY
- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
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- C—CHEMISTRY; METALLURGY
- 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
- C08K5/16—Nitrogen-containing compounds
- C08K5/34—Heterocyclic compounds having nitrogen in the ring
- C08K5/3467—Heterocyclic compounds having nitrogen in the ring having more than two nitrogen atoms in the ring
- C08K5/3477—Six-membered rings
- C08K5/3492—Triazines
- C08K5/34922—Melamine; Derivatives thereof
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- C—CHEMISTRY; METALLURGY
- 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
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D133/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Coating compositions based on derivatives of such polymers
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/08—Anti-corrosive paints
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/16—Antifouling paints; Underwater paints
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
- C09D7/62—Additives non-macromolecular inorganic modified by treatment with other compounds
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/63—Additives non-macromolecular organic
-
- C—CHEMISTRY; METALLURGY
- 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
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
Abstract
The invention relates to a preparation method of nano silicon dioxide-acrylic resin composite coating. The preparation method comprises the following steps: firstly, adding all solvents and about 1/5 of a mixed monomer dissolved with an initiator into a four-opening reaction bottle; starting to stir and heating the mixture to a reflowing temperature; starting to continuously dropwise add residual monomers; after a reaction is finished, adding a proper amount of triethylamine and neutralizing; cooling the mixture to be 40 DEG C or lower than 40 DEG C and discharging to obtain acrylic resin liquid; transferring a KH-570 raw solution into a beaker and adding distilled water and a few drops of oxalic acid solution; adjusting the pH value and stirring to dissolve; taking nano silicon dioxide, ethanol and a KH-570 water solution; pouring a formed suspension solution into a 200-mL three-necked bottle; after mixing acrylic resin with a methylated melamine curing agent and KH-570 modified silicon dioxide, adding a proper amount of flatting agent, de-foaming agent and other additives to obtain the coating. The method provided by the invention is simple and low in cost; the prepared nano silicon dioxide-acrylic resin composite coating has good dispersity and has relatively strong corrosion resistance and stain resistance.
Description
Technology neck and
The present invention relates to a kind of composite coating preparation method, particularly relate to the preparation method of a kind of nano silicon-acrylic resin composite coating.
Background technology
Current, stainless application development restricts to a great extent in its surface treatment and resist technology.Under the erosion action of various acid, caustic corrosion and wet environment, stainless surface property is subject to serious destruction.Use the method for coating protection effectively can protect the surface of steel plate, ostentatious effect can be played again, and have easy, cheap effect.In coating, add nano particle can obtain radioprotective, the ageing-resistant high-performance nano composite coating high with stripping strength.And nano composite dope is as a kind of new coating, there is good hardness, erosion resistance, pollution resistance, in stainless steel surface process and protection, there is larger actual value and practical significance.Bibliographical information nano silicon can increase hardness, the scoring resistance of film, can keep the transparency of film simultaneously.People generally adopt nano silicon to improve the mechanical property such as hardness, impact resistance, wear resistance of nano paint. the uv absorption property of nano silicon simultaneously, the very large ageing resistance that improve coating.Although the performance of the raising coating that silicon-dioxide can be larger, in preparation process, silicon-dioxide is easily reunited, and has a strong impact on the performance of coating. so the dispersion of nano silicon and modification are the key points preparing nano silicon composite coating.
Summary of the invention
It is simple that technical problem to be solved by this invention is to provide a kind of method, and with low cost, prepared nano silicon-acrylic resin composite coating good dispersity, has the preparation method of stronger anticorrosive and pollution resistance.
The technical scheme that the present invention solves the problems of the technologies described above is as follows: the preparation method of a kind of nano silicon-acrylic resin composite coating, is characterized in that, comprise the steps:
In four mouthfuls of reaction flasks, first add the mix monomer being dissolved with initiator of whole solvent and about 1/5;
Start stirring, be heated to reflux temperature, start to drip residual monomer continuously, reaction terminates, and adds the neutralization of appropriate triethylamine, is cooled to 40 DEG C with bottom discharge, obtains acrylic resin liquid;
Pipette KH-570 stoste and be placed in beaker, add distilled water and several oxalic acid solutions, adjust ph, stir and make it dissolve;
Get nano silicon, ethanol, and the KH-570 aqueous solution, by the suspension 200mL of the falling people three-necked bottle of formation;
By acrylic resin and melamine cured dose of methyl-etherified, add the appropriate flow agent of people, defoamer and other auxiliary agents after the silicon-dioxide mixing that KH-570 is modified and obtain coating.
On the basis of technique scheme, the present invention can also do following improvement.
Further, described in four mouthfuls of reaction flasks, first add whole solvent and about 1/5 be dissolved with being implemented as follows of the mixing single stage of initiator:
Adopting solution polymerization process, taking into account in four mouthfuls of reaction flasks of feeding device with agitator, reflux exchanger, temperature, first adding the mix monomer being dissolved with initiator of whole solvent and about 1/5.
Further, described in start stirring, be heated to reflux temperature, start drip residual monomer continuously, reaction terminate, add appropriate triethylamine neutralization, be cooled to 40 DEG C with bottom discharge, obtain being implemented as follows of acrylic resin liquid step:
Start stirring, be heated to reflux temperature, start to drip residual monomer continuously after insulation 45-60min, add in 2-3h; After insulation 1-1.5h, add second part of initiator, then be incubated 1h. inspection transformation efficiency and acid number, terminate when transformation efficiency >=98% reacts, add the neutralization of appropriate triethylamine, be cooled to 40 DEG C with bottom discharge, obtain acrylic resin liquid.
Further, described in pipette KH-570 stoste and be placed in beaker, add distilled water and several oxalic acid solutions, adjust ph, stir and make being implemented as follows of its dissolving step:
Pipette 5mLKH-570 stoste and be placed in beaker, add distilled water and several oxalic acid solutions, between adjust ph to 3.5 ~ 4, stir and make it dissolve.
Further, nano silicon is got, ethanol, and the KH-570 aqueous solution, by being implemented as follows of step in the suspension 200mL of the falling people three-necked bottle of formation described in:
Get nano silicon 5g, ethanol 100g, and the 2mLKH-570 aqueous solution, high speed shear 10min, rotating speed 2000r/min, by the suspension 200mL of the falling people three-necked bottle of formation, stir 6h at 50 DEG C.
The invention has the beneficial effects as follows: method is simple, and with low cost, prepared nano silicon-acrylic resin composite coating good dispersity, has stronger anticorrosive and pollution resistance.
Embodiment
Be described principle of the present invention and feature below in conjunction with example, example, only for explaining the present invention, is not intended to limit scope of the present invention.
A preparation method for nano silicon-acrylic resin composite coating, is characterized in that, comprise the steps:
In four mouthfuls of reaction flasks, first add the mix monomer being dissolved with initiator of whole solvent and about 1/5;
Start stirring, be heated to reflux temperature, start to drip residual monomer continuously, reaction terminates, and adds the neutralization of appropriate triethylamine, is cooled to 40 DEG C with bottom discharge, obtains acrylic resin liquid;
Pipette KH-570 stoste and be placed in beaker, add distilled water and several oxalic acid solutions, adjust ph, stir and make it dissolve;
Get nano silicon, ethanol, and the KH-570 aqueous solution, by the suspension 200mL of the falling people three-necked bottle of formation;
By acrylic resin and melamine cured dose of methyl-etherified, add the appropriate flow agent of people, defoamer and other auxiliary agents after the silicon-dioxide mixing that KH-570 is modified and obtain coating.
Embodiment 1:
Adopting solution polymerization process, taking into account in four mouthfuls of reaction flasks of feeding device with agitator, reflux exchanger, temperature, first adding the mix monomer being dissolved with initiator of whole solvent and about 1/5.Start stirring, be heated to reflux temperature, start to drip residual monomer continuously after insulation 45min, add in 2h; After insulation 1h, add second part of initiator, then be incubated 1h. inspection transformation efficiency and acid number, terminate when transformation efficiency >=98% reacts, add the neutralization of appropriate triethylamine, be cooled to 40 DEG C with bottom discharge, obtain acrylic resin liquid.Pipette 5mLKH-570 stoste and be placed in beaker, add distilled water and several oxalic acid solutions, between adjust ph to 3.5, stir and make it dissolve.Get nano silicon 5g, ethanol 100g, and the 2mLKH-570 aqueous solution, high speed shear 10min, rotating speed 2000r/min, by the suspension 200mL of the falling people three-necked bottle of formation, stir 6h at 50 DEG C.
Embodiment 2:
Adopting solution polymerization process, taking into account in four mouthfuls of reaction flasks of feeding device with agitator, reflux exchanger, temperature, first adding the mix monomer being dissolved with initiator of whole solvent and about 1/5.Start stirring, be heated to reflux temperature, start to drip residual monomer continuously after insulation 50min, add in 2.5h; After insulation 1.2h, add second part of initiator, then be incubated 1h. inspection transformation efficiency and acid number, terminate when transformation efficiency >=98% reacts, add the neutralization of appropriate triethylamine, be cooled to 40 DEG C with bottom discharge, obtain acrylic resin liquid.Pipette 5mLKH-570 stoste and be placed in beaker, add distilled water and several oxalic acid solutions, between adjust ph to 3.8, stir and make it dissolve.Get nano silicon 5g, ethanol 100g, and the 2mLKH-570 aqueous solution, high speed shear 10min, rotating speed 2000r/min, by the suspension 200mL of the falling people three-necked bottle of formation, stir 6h at 50 DEG C.
Embodiment 3:
Adopting solution polymerization process, taking into account in four mouthfuls of reaction flasks of feeding device with agitator, reflux exchanger, temperature, first adding the mix monomer being dissolved with initiator of whole solvent and about 1/5.Start stirring, be heated to reflux temperature, start to drip residual monomer continuously after insulation 60min, add in 3h; After insulation 1.5h, add second part of initiator, then be incubated 1h. inspection transformation efficiency and acid number, terminate when transformation efficiency >=98% reacts, add the neutralization of appropriate triethylamine, be cooled to 40 DEG C with bottom discharge, obtain acrylic resin liquid.Pipette 5mLKH-570 stoste and be placed in beaker, add distilled water and several oxalic acid solutions, between adjust ph to 4, stir and make it dissolve.Get nano silicon 5g, ethanol 100g, and the 2mLKH-570 aqueous solution, high speed shear 10min, rotating speed 2000r/min, by the suspension 200mL of the falling people three-necked bottle of formation, stir 6h at 50 DEG C.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (5)
1. a preparation method for nano silicon-acrylic resin composite coating, is characterized in that, comprise the steps:
In four mouthfuls of reaction flasks, first add the mix monomer being dissolved with initiator of whole solvent and about 1/5;
Start stirring, be heated to reflux temperature, start to drip residual monomer continuously, reaction terminates, and adds the neutralization of appropriate triethylamine, is cooled to 40 DEG C with bottom discharge, obtains acrylic resin liquid;
Pipette KH-570 stoste and be placed in beaker, add distilled water and several oxalic acid solutions, adjust ph, stir and make it dissolve;
Get nano silicon, ethanol, and the KH-570 aqueous solution, by the suspension 200mL of the falling people three-necked bottle of formation;
By acrylic resin and melamine cured dose of methyl-etherified, add the appropriate flow agent of people, defoamer and other auxiliary agents after the silicon-dioxide mixing that KH-570 is modified and obtain coating.
2. the preparation method of a kind of nano silicon-acrylic resin composite coating according to claim 1, is characterized in that, described in four mouthfuls of reaction flasks, first add whole solvent and about 1/5 be dissolved with being implemented as follows of the mixing single stage of initiator:
Adopting solution polymerization process, taking into account in four mouthfuls of reaction flasks of feeding device with agitator, reflux exchanger, temperature, first adding the mix monomer being dissolved with initiator of whole solvent and about 1/5.
3. the preparation method of a kind of nano silicon-acrylic resin composite coating according to claim 1, it is characterized in that, describedly start stirring, be heated to reflux temperature, start to drip residual monomer continuously, reaction terminates, and adds the neutralization of appropriate triethylamine, be cooled to 40 DEG C with bottom discharge, obtain being implemented as follows of acrylic resin liquid step:
Start stirring, be heated to reflux temperature, start to drip residual monomer continuously after insulation 45-60min, add in 2-3h; After insulation 1-1.5h, add second part of initiator, then be incubated 1h. inspection transformation efficiency and acid number, terminate when transformation efficiency >=98% reacts, add the neutralization of appropriate triethylamine, be cooled to 40 DEG C with bottom discharge, obtain acrylic resin liquid.
4. the preparation method of a kind of nano silicon-acrylic resin composite coating according to claim 1, it is characterized in that, described in pipette KH-570 stoste and be placed in beaker, add distilled water and several oxalic acid solutions, adjust ph, stirs and makes being implemented as follows of its dissolving step:
Pipette 5mLKH-570 stoste and be placed in beaker, add distilled water and several oxalic acid solutions, between adjust ph to 3.5 ~ 4, stir and make it dissolve.
5. the preparation method of a kind of nano silicon-acrylic resin composite coating according to claim 1, it is characterized in that, described in get nano silicon, ethanol, and the KH-570 aqueous solution, by being implemented as follows of step in the suspension 200mL of the falling people three-necked bottle of formation:
Get nano silicon 5g, ethanol 100g, and the 2mLKH-570 aqueous solution, high speed shear 10min, rotating speed 2000r/min, by the suspension 200mL of the falling people three-necked bottle of formation, stir 6h at 50 DEG C.
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| CN201510992028.2A CN105482585A (en) | 2015-12-25 | 2015-12-25 | Preparation method of nano silicon dioxide-acrylic resin composite coating |
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| CN201510992028.2A CN105482585A (en) | 2015-12-25 | 2015-12-25 | Preparation method of nano silicon dioxide-acrylic resin composite coating |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106566354A (en) * | 2016-11-11 | 2017-04-19 | 浙江大学 | Nano composite anti-fouling paint co-used with anticorrosion intermediate paint and preparation method thereof |
| CN109486344A (en) * | 2018-09-30 | 2019-03-19 | 镇江宝海船舶五金有限公司 | A kind of antibacterial epoxy coating of anchor chain and preparation method thereof |
| CN111793406A (en) * | 2020-08-03 | 2020-10-20 | 百氏高涂料（苏州）有限公司 | Corrosion-resistant high-molecular nano hydrophilic coating and preparation method thereof |
| CN114702871A (en) * | 2022-05-18 | 2022-07-05 | 深圳市恒辉纳米科技有限公司 | Metal surface oil-stain-resistant nano coating agent and preparation method thereof |
-
2015
- 2015-12-25 CN CN201510992028.2A patent/CN105482585A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106566354A (en) * | 2016-11-11 | 2017-04-19 | 浙江大学 | Nano composite anti-fouling paint co-used with anticorrosion intermediate paint and preparation method thereof |
| CN106566354B (en) * | 2016-11-11 | 2019-02-19 | 浙江大学 | With the matching used nano combined antifouling paint of anti-corrosion intermediate coat and preparation method thereof |
| CN109486344A (en) * | 2018-09-30 | 2019-03-19 | 镇江宝海船舶五金有限公司 | A kind of antibacterial epoxy coating of anchor chain and preparation method thereof |
| CN111793406A (en) * | 2020-08-03 | 2020-10-20 | 百氏高涂料（苏州）有限公司 | Corrosion-resistant high-molecular nano hydrophilic coating and preparation method thereof |
| CN114702871A (en) * | 2022-05-18 | 2022-07-05 | 深圳市恒辉纳米科技有限公司 | Metal surface oil-stain-resistant nano coating agent and preparation method thereof |
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Application publication date: 20160413 |
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