CN110437698B - Water-based environment-friendly coating and preparation method thereof - Google Patents
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- C09D143/00—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 containing boron, silicon, phosphorus, selenium, tellurium, or a metal; Coating compositions based on derivatives of such polymers
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- C09D7/40—Additives
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Abstract
The invention relates to a water-based environment-friendly coating and a preparation method thereof, belonging to the field of coatings. The water-based environment-friendly coating is prepared by taking organic silicon modified acrylic latex as a main component and matching with inorganic filler and other auxiliary agents. The carbon nano tube and the nano silicon dioxide which are modified by alkylation are used as inorganic fillers, and the carbon nano tube and the nano silicon dioxide are jointly used, so that the point and line synergistic enhancement can be formed, when the coating is very thin, a uniform and smooth film can be formed, the carbon nano tube and the nano silicon dioxide which are modified by alkylation can effectively avoid the agglomeration of the fillers, and the dispersibility of the inorganic fillers in coating resin is effectively improved. The alkylation modified filler has the function of a defoaming agent, so that other defoaming agents are not required to be added into the water-based environment-friendly coating. The water-based environment-friendly coating prepared by the invention has excellent mechanical property, adhesive force, hydrophilicity and water resistance. The preparation method is simple and feasible, has good stability and good repeatability, and is easy to realize industrial production.
Description
Technical Field
The invention relates to a preparation method of a coating, in particular to a water-based environment-friendly coating and a preparation method thereof, belonging to the field of coatings.
Background
The paint is a high molecular material which is widely used for coating the surfaces of various base materials. One important function of the coating is protection, and the organic coating is coated on the surface of metal and can isolate the metal from being contacted with oxygen and water, so that the metal is protected from various damages and corrosion. The paint also plays an important role in indicating signs, and different marked signboards and road separation lines on roads, and various pipes and equipment with different colors in factories represent different functions and effects through different colors of the paint. Coatings have been developed to date and are widely classified into solvent-borne coatings and solventless coatings, and solvent-borne coatings and water-borne coatings. The solvent-based paint contains a large amount of VOC, when the paint is cured into a film, the solvent is volatilized into the air, so that the environment is polluted, the human health is influenced, and people gradually realize that the organic solvent in the paint can cause irreversible damage to the nature along with the higher and higher environmental protection requirements of the state on the chemical industry. Therefore, the development and use of the water-based paint are more in line with the requirements of social sustainable development and human health growth.
The aqueous coating materials can be classified into aqueous acrylic coatings, aqueous epoxy resin coatings, aqueous polyurethane coatings, aqueous alkyd resin coatings, and the like according to the difference of film-forming materials in the aqueous coating materials. The acrylic resin has good gloss and color retention, weather resistance, corrosion resistance and film forming property, is convenient and simple to produce and construct, and has no pollution to the environment, so that the acrylic resin is applied to water-based paint in many ways, and is one of hot spots for the research of the paint and adhesive industry. However, the decorative properties of the above coatings on the substrate are still poor, and the adhesion cannot meet high requirements, which limits further applications. Therefore, it is necessary to invent a water-based environment-friendly coating with good performance and a preparation method thereof.
Disclosure of Invention
The invention provides a water-based environment-friendly coating for overcoming the defects of the prior art, and the coating has excellent mechanical property, adhesive force, hydrophilicity and water resistance. The water-based environment-friendly coating is prepared from the following raw materials in parts by weight:
50-70 parts of organic silicon modified acrylic latex;
20-35 parts of an alkylation modified filler;
10-20 parts of a leveling agent;
20-30 parts of water.
The organic silicon modified acrylic latex is quadripolymer latex of methyl acrylate, acryloyl morpholine, hydroxyethyl acrylate and vinyl trimethoxy silane, and the molecular weight is 4000-10000.
Wherein the organosilicon modified acrylic latex is prepared by the following steps:
adding sodium dodecyl sulfate and allyl octyl phenol polyoxyethylene ether into a reaction kettle in sequence, fully dissolving the sodium dodecyl sulfate and the allyl octyl phenol polyoxyethylene ether by using deionized water, slowly adding monomer mixed liquid (the monomer mixed liquid comprises methyl acrylate, acryloyl morpholine, hydroxyethyl acrylate and vinyl trimethoxy silane) while stirring, and fully stirring to obtain the pre-emulsion. And slowly adding 3-5 wt% of ammonium sulfate aqueous solution with the total weight of 1-2% into the pre-emulsion, and controlling the speed to finish feeding within 1-1.5 h. And then raising the temperature of the system to 80-85 ℃, and reacting for 4-5.5 h to obtain the organic silicon modified acrylic latex.
Preferably, the mass ratio of the sodium dodecyl sulfate to the allyl octyl phenol polyoxyethylene ether to the deionized water is 1: 1-1.2: 3-6.
Preferably, the molar ratio of the methyl acrylate, the acryloyl morpholine, the hydroxyethyl acrylate and the vinyl trimethoxy silane is 2:1:1: 1.
Preferably, the ratio of sodium lauryl sulfate: the molar ratio of the methyl acrylate is 1: 0.3-0.5.
Wherein the alkylation modified filler is a mixture of alkylated carbon nanotubes and alkylated nano-silica.
Wherein the alkylated modified filler is prepared by the following steps:
uniformly mixing the carbon nano tube and the nano silicon dioxide according to the weight ratio of 1:1, placing the mixture in a vacuum drying oven for vacuum degassing for 1-2 hours, removing free moisture, transferring the degassed filler into a reaction kettle filled with inert gas through an internal transfer method, adding 40-50 wt% of vinyl trimethoxy silane ethanol solution, reacting for 2-4 hours at 110-120 ℃, stopping the reaction, filtering and drying to obtain the alkylated modified filler consisting of a mixture of the alkylated carbon nano tube and the alkylated silicon dioxide. The alkylated and modified filler has good dispersibility in the organosilicon acrylic latex and the water dispersion medium.
Preferably, the carbon nanotube is a multi-walled carbon nanotube, the inner diameter is 5-10 nm, the outer diameter is 10-20 nm, and the length is 10-25 nm.
Preferably, the mass ratio of the nano silicon dioxide to the vinyl trimethoxy silane is 1: 2.6-3.2.
Preferably, the leveling agent is selected from one or more of polyvinyl butyral, polydimethylsiloxane and diacetone alcohol.
The preparation method of the water-based environment-friendly coating comprises the following steps:
(1) weighing 50-70 parts of organic silicon modified acrylic latex, 10-20 parts of flatting agent and 20-30 parts of water, mixing in a stirrer, stirring and mixing for 1-1.5 h at the temperature of 45-50 ℃ and the rotating speed of 500-600 r/min, and stopping.
(2) And (3) ultrasonically dispersing 20-35 parts of the alkylated modified filler, adding into the mixture, stirring and mixing at the rotating speed of 500-600 r/min at room temperature for 30-40 min, and stopping.
(3) And (3) adjusting the pH value of the mixture obtained in the step (2) to be neutral by using ammonia water, and then grinding and mixing the mixture by using a conical mill to obtain the water-based environment-friendly coating.
(4) When in use, 0.5-1.5 wt% of triethylene tetramine curing agent is added, and after uniform mixing, coating is carried out.
The beneficial effects are as follows:
1. the water-based environment-friendly coating is prepared by taking organic silicon modified acrylic latex as a main component and matching with inorganic filler and other auxiliary agents, the acrylate copolymer has good hydrophilicity but poor water resistance, and the water resistance is improved by modification of organic silicon.
2. The water-based environment-friendly coating takes the alkylated modified carbon nano tube and the nano silicon dioxide as inorganic fillers, and the carbon nano tube in the shape of nano fiber can form an interweaving layer in the coating, so that the coating has obvious effects of strengthening and toughening. The combined use of carbon nanotubes and nanosilica can form a synergistic enhancement of dots and lines, and a uniform, smooth film can be formed when the coating is thin. In addition, the carbon nano tube and the nano silicon dioxide which are subjected to alkylation modification can effectively avoid the agglomeration of the filler, and effectively improve the dispersibility of the inorganic filler in the coating resin.
3. The added alkylation modified filler has the function of a defoaming agent, so that other defoaming agents are not needed to be added into the water-based environment-friendly coating.
4. The water-based environment-friendly coating prepared by the invention has excellent mechanical property, adhesive force, hydrophilicity and water resistance. The preparation method is simple and feasible, has good stability and good repeatability, and is easy to realize industrial production.
Detailed Description
The present invention will be further described with reference to specific examples, which are not intended to limit the invention.
Example 1
The invention provides a water-based environment-friendly coating which is prepared from the following raw materials in parts by weight:
50 parts of organic silicon modified acrylic latex;
20 parts of an alkylation modified filler;
5 parts of polyvinyl butyral;
5 parts of polydimethylsiloxane;
and 20 parts of water.
The preparation method of the water-based environment-friendly coating comprises the following steps:
(1) preparation of the silicone-modified acrylic latex: 12.5kg of sodium dodecyl sulfate and 12.5kg of allyl octyl phenol polyoxyethylene ether are sequentially added into a reaction kettle, and are fully dissolved by 37.5kg of deionized water, and a monomer mixed solution (the monomer mixed solution comprises 0.83kg of methyl acrylate, 0.68kg of acryloyl morpholine, 0.56kg of hydroxyethyl acrylate and 0.72kg of vinyl trimethoxy silane) is slowly added while stirring, and is fully stirred to obtain a pre-emulsion. 0.65kg of 3-5 wt% ammonium sulfate aqueous solution is slowly added into the pre-emulsion, and the feeding is finished within 1 hour under the control of the speed. And then raising the temperature of the system to 80 ℃, and reacting for 5.5 hours to obtain the organic silicon modified acrylic latex.
(2) Preparing an alkylated modified filler:
uniformly mixing 1.2kg of carbon nano tube and 1.2kg of nano silicon dioxide, placing the mixture in a vacuum drying oven for vacuum degassing for 1h to remove free moisture, transferring the degassed filler into a reaction kettle filled with inert gas by an internal transfer method, adding 3.9kg of 40wt% ethanol solution of vinyl trimethoxy silane, reacting for 2h at 110 ℃, filtering and drying after the reaction is stopped, and obtaining the alkylated modified filler consisting of the mixture of the alkylated carbon nano tube and the alkylated silicon dioxide. The alkylated and modified filler has good dispersibility in the organosilicon acrylic latex and the water dispersion medium. The carbon nano tube is a multi-wall carbon nano tube, the inner diameter is 5-10 nm, the outer diameter is 10-20 nm, and the length is 10-25 nm.
(3) 50 parts of organic silicon modified acrylic latex, 5 parts of polyvinyl butyral, 5 parts of polydimethylsiloxane and 20 parts of water are mixed in a stirrer, and the stirring and the mixing are stopped after 1 hour at the temperature of 45 ℃ and the rotating speed of 500 r/min.
(4) And (3) ultrasonically dispersing 20 parts of the alkylated modified filler, adding the mixture into the mixture, stirring and mixing at the rotation speed of 550r/min at room temperature for 30min, and stopping.
(5) And (4) adjusting the pH value of the mixture obtained in the step (4) to be neutral by using ammonia water, and then grinding and mixing the mixture by using a conical mill to obtain the water-based environment-friendly coating.
(6) When in use, the triethylene tetramine curing agent with the total weight of 0.5wt% is added, and the coating is carried out after the uniform mixing.
Example 2
The invention provides a water-based environment-friendly coating which is prepared from the following raw materials in parts by weight:
60 parts of organosilicon modified acrylic latex;
28 parts of an alkylation modified filler;
5 parts of polyvinyl butyral;
5 parts of polydimethylsiloxane;
5 parts of diacetone alcohol;
and 25 parts of water.
The preparation method of the water-based environment-friendly coating comprises the following steps:
(1) preparation of the silicone-modified acrylic latex: 12.5kg of lauryl sodium sulfate and 13.2kg of allyl octyl phenol polyoxyethylene ether are sequentially added into a reaction kettle, 49kg of deionized water is used for full dissolution, monomer mixed liquid (the monomer mixed liquid comprises 1.11kg of methyl acrylate, 0.91kg of acryloyl morpholine, 0.75kg of hydroxyethyl acrylate and 0.96kg of vinyl trimethoxy silane) is slowly added while stirring, and full stirring is carried out to obtain pre-emulsion. 1.18kg of 3-5 wt% ammonium sulfate aqueous solution is slowly added into the pre-emulsion, and the feeding is finished within 1 hour under the control of the speed. And then raising the temperature of the system to 85 ℃, and reacting for 4 hours to obtain the organic silicon modified acrylic latex.
(2) Preparing an alkylated modified filler:
uniformly mixing 1.2kg of carbon nano tube and 1.2kg of nano silicon dioxide, placing the mixture in a vacuum drying oven for vacuum degassing for 1.5h, removing free moisture, transferring the degassed filler into a reaction kettle filled with inert gas by an internal transfer method, adding 4.0kg of 45wt% vinyl trimethoxy silane ethanol solution, reacting for 3h at 115 ℃, filtering and drying after the reaction is stopped, and obtaining the alkylation modified filler consisting of the mixture of the alkylation carbon nano tube and the alkylation silicon dioxide. The alkylated and modified filler has good dispersibility in the organosilicon acrylic latex and the water dispersion medium. The carbon nano tube is a multi-wall carbon nano tube, the inner diameter is 5-10 nm, the outer diameter is 10-20 nm, and the length is 10-25 nm.
(3) 60 parts of organic silicon modified acrylic latex, 5 parts of polyvinyl butyral, 5 parts of polydimethylsiloxane, 5 parts of diacetone alcohol and 25 parts of water are weighed and mixed in a stirrer, and the stirring and mixing are stopped after 1.5 hours under the conditions that the temperature is 50 ℃ and the rotating speed is 600 r/min.
(4) And (3) ultrasonically dispersing 28 parts of the alkylated modified filler, adding the mixture into the mixture, stirring and mixing at the rotating speed of 600r/min at room temperature for 35min, and stopping.
(5) And (4) adjusting the pH value of the mixture obtained in the step (4) to be neutral by using ammonia water, and then grinding and mixing the mixture by using a conical mill to obtain the water-based environment-friendly coating.
(6) When in use, the triethylene tetramine curing agent with the total weight of 1.0wt% is added, and the coating is carried out after the uniform mixing.
Example 3
The invention provides a water-based environment-friendly coating which is prepared from the following raw materials in parts by weight:
70 parts of organosilicon modified acrylic latex;
35 parts of an alkylation modified filler;
9 parts of polyvinyl butyral;
11 parts of diacetone alcohol;
and 30 parts of water.
The preparation method of the water-based environment-friendly coating comprises the following steps:
(1) preparation of the silicone-modified acrylic latex: 12.5kg of sodium dodecyl sulfate and 15kg of allyl octyl phenol polyoxyethylene ether are sequentially added into a reaction kettle, 75kg of deionized water is used for fully dissolving, monomer mixed liquor (the monomer mixed liquor comprises 1.39kg of methyl acrylate, 1.14kg of acryloyl morpholine, 0.94kg of hydroxyethyl acrylate and 1.20kg of vinyl trimethoxy silane) is slowly added while stirring, and the pre-emulsion is obtained after full stirring. 2.14kg of 3-5 wt% ammonium sulfate aqueous solution is slowly added into the pre-emulsion, and the feeding is finished within 1.5 h. And then raising the temperature of the system to 82 ℃, and reacting for 5 hours to obtain the organosilicon modified acrylic latex.
(2) Uniformly mixing 1.2kg of carbon nano tube and 1.2kg of nano silicon dioxide, placing the mixture in a vacuum drying oven for vacuum degassing for 2h, removing free moisture, transferring the degassed filler into a reaction kettle filled with inert gas by an internal transfer method, adding 3.84kg of 50wt% vinyl trimethoxy silane ethanol solution, reacting for 4h at 120 ℃, stopping the reaction, filtering and drying to obtain the alkylated modified filler consisting of the mixture of the alkylated carbon nano tube and the alkylated silicon dioxide. The alkylated and modified filler has good dispersibility in the organosilicon acrylic latex and the water dispersion medium. The carbon nano tube is a multi-wall carbon nano tube, the inner diameter is 5-10 nm, the outer diameter is 10-20 nm, and the length is 10-25 nm.
(1) Weighing 70 parts of organic silicon modified acrylic latex, 9 parts of polyvinyl butyral, 11 parts of diacetone alcohol and 30 parts of water, mixing in a stirrer, stirring and mixing for 1.5h at the temperature of 50 ℃ and the rotating speed of 600r/min, and stopping.
(2) And adding 35 parts of the alkylated modified filler into the mixture after ultrasonic dispersion, stirring and mixing at the rotating speed of 600r/min at room temperature for 40min, and stopping.
(3) And (3) adjusting the pH value of the mixture obtained in the step (2) to be neutral by using ammonia water, and then grinding and mixing the mixture by using a conical mill to obtain the water-based environment-friendly coating.
(4) When in use, the triethylene tetramine curing agent with the total weight of 1.5wt% is added, and the coating is carried out after the uniform mixing.
Comparative example 1
The procedure of example 1 was repeated except that the commercially available acrylic resin was used instead of the silicone-modified acrylic latex.
Comparative example 2
The same procedure as in example 1 was repeated except that the alkylated carbon nanotubes were replaced with the same mass of alkylated nano-silica.
Comparative example 3
The same procedure as in example 1 was repeated except that the alkylated nano-silica was replaced with the same mass of alkylated carbon nanotube.
And (4) comparing the results:
the tensile property is tested by a universal material testing machine according to ASTM D638 and ASTM D790 test standards, the pencil hardness is tested by GB/T6739-.
The silicone-modified acrylic latex has excellent toughness and water resistance, and when the acrylic latex is replaced with a commercially available acrylic resin, the hardness, elongation at break, tensile strength, impact strength and adhesion are all reduced, and the water resistance is reduced, as shown in comparative example 1. When the alkylated carbon nanotube and the alkylated nano-silica are used as inorganic fillers at the same time, the alkylated carbon nanotube and the alkylated nano-silica show better mechanical properties, and when the alkylated carbon nanotube and the alkylated nano-silica are used independently, impact strength, adhesive force, tensile strength and elongation at break are influenced, see comparative example 2 and comparative example 3.
In conclusion, the water-based environment-friendly coating disclosed by the invention is environment-friendly, does not use an organic solvent, and has excellent mechanical properties and water resistance.
Claims (6)
1. The water-based environment-friendly coating is characterized by being prepared from the following raw materials in parts by weight:
50-70 parts of organic silicon modified acrylic latex;
20-35 parts of an alkylation modified filler;
10-20 parts of a leveling agent;
20-30 parts of water;
wherein the organic silicon modified acrylic latex is quadripolymer latex of methyl acrylate, acryloyl morpholine, hydroxyethyl acrylate and vinyl trimethoxy silane, and the molecular weight is 4000-10000;
the organic silicon modified acrylic latex is prepared by the following steps: sequentially adding sodium dodecyl sulfate and allyl octyl phenol polyoxyethylene ether into a reaction kettle, fully dissolving the sodium dodecyl sulfate and the allyl octyl phenol polyoxyethylene ether by using deionized water, slowly adding a monomer mixed solution of methyl acrylate, acryloyl morpholine, hydroxyethyl acrylate and vinyl trimethoxy silane while stirring, and fully stirring to obtain a pre-emulsion; slowly adding 3-5 wt% of ammonium persulfate aqueous solution with the total weight of 1-2% into the pre-emulsion, and controlling the speed to finish the feeding within 1-1.5 h; then, raising the temperature of the system to 80-85 ℃, and reacting for 4-5.5 hours to obtain the organic silicon modified acrylic latex;
wherein the alkylated modified filler is a mixture of alkylated carbon nanotubes and alkylated nano-silica; the alkylated modified filler is prepared by the following steps: uniformly mixing the carbon nano tube and the nano silicon dioxide according to the weight ratio of 1:1, placing the mixture in a vacuum drying oven for vacuum degassing for 1-2 hours, removing free moisture, transferring the degassed filler into a reaction kettle filled with inert gas through an internal transfer method, adding 40-50 wt% of vinyl trimethoxy silane ethanol solution, reacting for 2-4 hours at 110-120 ℃, stopping the reaction, filtering and drying to obtain the alkylated modified filler consisting of a mixture of the alkylated carbon nano tube and the alkylated silicon dioxide.
2. The aqueous environment-friendly coating as claimed in claim 1, wherein: the mass ratio of the sodium dodecyl sulfate to the allyl octyl phenol polyoxyethylene ether to the deionized water is 1: 1-1.2: 3-6.
3. The aqueous environment-friendly coating as claimed in claim 1, wherein: the molar ratio of the methyl acrylate to the acryloyl morpholine to the hydroxyethyl acrylate to the vinyl trimethoxy silane is 2:1:1: 1.
4. The aqueous environment-friendly coating as claimed in claim 1, wherein: the sodium dodecyl sulfate: the molar ratio of the methyl acrylate is 1: 0.3-0.5.
5. The aqueous environment-friendly coating as claimed in claim 1, wherein: the carbon nano tube is a multi-wall carbon nano tube, the inner diameter is 5-10 nm, the outer diameter is 10-20 nm, and the length is 10-25 nm; the mass ratio of the nano silicon dioxide to the vinyl trimethoxy silane is 1: 2.6-3.2; the leveling agent is selected from one or more of polyvinyl butyral, polydimethylsiloxane and diacetone alcohol.
6. A method for preparing the aqueous environmental protection coating according to claim 1, comprising the steps of:
1) weighing 50-70 parts of organic silicon modified acrylic latex, 10-20 parts of flatting agent and 20-30 parts of water, mixing in a stirrer, stirring and mixing for 1-1.5 h at the temperature of 45-50 ℃ and the rotating speed of 500-600 r/min, and stopping;
2) adding 20-35 parts of the alkylated modified filler into the mixture after ultrasonic dispersion, stirring and mixing at the rotating speed of 500-600 r/min at room temperature for 30-40 min, and stopping;
3) adjusting the pH value of the mixture obtained in the step 2) to be neutral by using ammonia water, and then grinding and mixing the mixture by using a conical mill to obtain the water-based environment-friendly coating; when in use, 0.5-1.5 wt% of triethylene tetramine curing agent is added, and after uniform mixing, coating is carried out.
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