CN113024821A - Water-based alkyd acrylic hybrid resin and preparation method thereof - Google Patents
Water-based alkyd acrylic hybrid resin and preparation method thereof Download PDFInfo
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- CN113024821A CN113024821A CN202110234275.1A CN202110234275A CN113024821A CN 113024821 A CN113024821 A CN 113024821A CN 202110234275 A CN202110234275 A CN 202110234275A CN 113024821 A CN113024821 A CN 113024821A
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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
- C08G81/00—Macromolecular compounds obtained by interreacting polymers in the absence of monomers, e.g. block polymers
- C08G81/02—Macromolecular compounds obtained by interreacting polymers in the absence of monomers, e.g. block polymers at least one of the polymers being obtained by reactions involving only carbon-to-carbon unsaturated bonds
- C08G81/024—Block or graft polymers containing sequences of polymers of C08C or C08F and of polymers of C08G
- C08G81/027—Block or graft polymers containing sequences of polymers of C08C or C08F and of polymers of C08G containing polyester or polycarbonate sequences
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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
- C09D187/00—Coating compositions based on unspecified macromolecular compounds, obtained otherwise than by polymerisation reactions only involving unsaturated carbon-to-carbon bonds
- C09D187/005—Block or graft polymers not provided for in groups C09D101/00 - C09D185/04
Abstract
The invention belongs to the technical field of high-performance environment-friendly coatings, and discloses a water-based alkyd acrylic hybrid resin and a preparation method thereof. The coating prepared from the water-based alkyd acrylic hybrid resin has excellent water resistance, dryness, hardness, heat storage capacity and other properties, and the water-based paint prepared from the resin combines the excellent wettability of alkyd resin and acrylic acid and the bearing capacity of pigments and fillers, has the gloss of 85-90 and is suitable for the large-scale civil paint field and the industrial paint field.
Description
Technical Field
The invention relates to the technical field of high-performance environment-friendly coatings, in particular to a water-based alkyd acrylic hybrid resin and a preparation method thereof.
Background
With the development of industry, the problem of environmental pollution is more and more troubling human beings, so the development of environment-friendly coatings is a great trend. The fundamental approach to solve the problem of environmental pollution from coatings is to develop solventless coatings, water-borne coatings, powder coatings and high solids coatings. With the enhancement of environmental awareness and the stricter environmental regulations, the water-based paint has become one of the main development directions of the environmental-friendly paint, and the water-based paint reduces the environmental pollution because all or most of water replaces the organic solvent.
The alkyd resin is an important resin for paint, and has the advantages of abundant monomer sources, low price, multiple varieties, large formula change, convenience for chemical modification and good performance; the alkyd resin can be used for preparing single-component self-drying paint, or can be used for preparing two-component self-drying (such as polyurethane paint) or amino baking paint. Alkyd resins have therefore always taken an important position in the coatings industry since their development.
However, like other solvent-based coatings, solvent-based alkyd coatings contain a large amount of solvent (> 25%), and are therefore a serious hazard to the atmospheric environment and to the health of operators during production and construction. In addition, due to the defect that an ester group in the molecular structure of the alkyd resin is easy to hydrolyze, the water resistance of the alkyd resin is poor, and meanwhile, the waterborne alkyd resin after air drying has the defect that a paint film is soft, so that the application range and development space of the waterborne alkyd resin are limited.
The acrylic resin has the advantages of excellent water resistance and adjustable paint film hardness, so that the development of the water-based alkyd acrylic hybrid resin with excellent water resistance has important significance.
Disclosure of Invention
The invention aims to provide a water-based alkyd acrylic hybrid resin and a preparation method thereof, and solves the problem that when the existing chemically modified water-based alkyd resin is used for preparing water-based paint, the water resistance and other properties of the existing chemically modified water-based alkyd resin are low.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a water-based alkyd acrylic hybrid resin which comprises the following raw materials in parts by weight:
15-35 parts of fatty acid modified acrylic prepolymer, 15-35 parts of basic alkyd resin, 1-12 parts of solvent, 1-5 parts of neutralizer and 35-55 parts of water;
the fatty acid modified acrylic prepolymer is prepared from the following raw materials in parts by weight: 1-50 parts of fatty acid, 1-99 parts of (methyl) acrylic acid and ester monomers thereof, 1-50 parts of vinyl monomers, 1-15 parts of double-bond-containing anhydride or dibasic acid, 10-30 parts of solvent and 0.5-5 parts of initiator;
the basic alkyd resin is prepared from the following raw materials in parts by weight: 30-70 parts of fatty acid, 10-40 parts of polybasic acid, 10-40 parts of polyalcohol, 1-15 parts of monobasic acid, 0.1-1 part of antioxidant, 0.1-1 part of catalyst and 2-10 parts of solvent;
the solvent is one or more of ethylene glycol butyl ether, propylene glycol methyl ether, propylene glycol butyl ether, xylene, S100 solvent, n-butanol and isopropanol;
the neutralizing agent is one or more of triethylamine, ammonia water and dimethylethanolamine.
Preferably, in the above one waterborne alkyd acrylic hybrid resin, the fatty acid is one or more of linolenic acid, linoleic acid, eleostearic acid, soya oleic acid, tall oil fatty acid and oleic acid.
Preferably, in one of the above-mentioned aqueous alkyd acrylic hybrid resins, the (methyl) acrylic acid and the ester monomer thereof are one or more of isooctyl acrylate, acrylic acid, isobornyl acrylate, n-butyl acrylate, methyl acrylate, ethyl acrylate, n-octyl acrylate, ethoxyethoxyethoxyethyl acrylate, 2-hydroxyethyl acrylate, 2-hydroxypropyl acrylate, methyl methacrylate, methacrylic acid, isobutyl methacrylate, octadecyl methacrylate, acetoacetoxy methacrylate, glycidyl methacrylate, isooctyl methacrylate, gamma-methacryloxypropyltriisopropoxysilane, gamma-methacryloxypropyltrimethoxysilane, gamma-methacryloxypropyltriethoxysilane and lauryl methacrylate.
Preferably, in one of the above water-based alkyd acrylic hybrid resins, the vinyl monomer is one or more of styrene, alpha-methyl styrene, vinyltrimethoxysilane, vinyltriethoxysilane and vinyltriisopropoxysilane.
Preferably, in one of the above water-based alkyd acrylic hybrid resins, the double bond-containing anhydride or dibasic acid is one or more of maleic anhydride, tetrahydrophthalic anhydride, maleic acid, fumaric acid and itaconic acid.
Preferably, in one of the above waterborne alkyd acrylic hybrid resins, the initiator is tert-butyl peroxybenzoate or di-tert-amyl peroxide.
Preferably, in one of the above water-based alkyd acrylic hybrid resins, the polybasic acid is one or more of phthalic anhydride, isophthalic acid, terephthalic acid, tetrahydrophthalic anhydride and adipic acid.
Preferably, in one of the above waterborne alkyd acrylic hybrid resins, the polyol is one or more of glycerol, trimethylolpropane, ethylene glycol, neopentyl glycol and pentaerythritol.
Preferably, in one of the above water-borne alkyd acrylic hybrid resins, the monoacid is benzoic acid.
Preferably, in the above waterborne alkyd acrylic hybrid resin, the antioxidant is triphenyl phosphite or hypophosphorous acid.
Preferably, in one of the above waterborne alkyd acrylic hybrid resins, the catalyst is titanate or triphenylphosphine.
The invention also provides a preparation method of the water-based alkyd acrylic hybrid resin, which comprises the following steps:
mixing the fatty acid modified acrylic prepolymer and the basic alkyd resin, heating to the temperature of 175-185 ℃ for esterification reaction, ending the reaction when the acid value is 20-50mgKOH/g, cooling to the temperature of 110-120 ℃, adding the solvent, continuously cooling to the temperature of 70-80 ℃, adding the neutralizing agent, and then adding water for dilution to obtain the water-based alkyd acrylic hybrid resin; wherein the mass of the solid of the water-based alkyd acrylic hybrid resin is 30-50%.
Preferably, in the above preparation method of the waterborne alkyd acrylic hybrid resin, the preparation method of the fatty acid modified acrylic prepolymer is as follows:
mixing fatty acid, (methyl) acrylic acid and ester monomers thereof, vinyl monomers, double-bond-containing acid anhydride or dibasic acid and an initiator, dripping the mixture into a solvent in multiple steps, and reacting at constant temperature for 1-3 hours after finishing dripping to obtain a fatty acid modified acrylic prepolymer; wherein the dropping time is 3-9h, and the temperature in the dropping process is 110-150 ℃.
Preferably, in the above preparation method of the water-based alkyd acrylic hybrid resin, the preparation method of the base alkyd resin is as follows:
mixing fatty acid, polybasic acid, polyalcohol, monobasic acid, antioxidant, catalyst and solvent, heating to 185 ℃ in nitrogen atmosphere, reacting at constant temperature for 1h, continuously heating to 225 ℃ at constant temperature, reacting at constant temperature until the solution becomes clear and transparent, heating to 250 ℃ at constant temperature at 245 ℃, reacting at constant temperature until the acid value is less than 10mgKOH/g, cooling, diluting boiled water and solvent, and discharging to obtain the basic alkyd resin.
Preferably, in the above preparation method of a waterborne alkyd acrylic hybrid resin, the fatty acid modified acrylic prepolymer is a fatty acid modified acrylic prepolymer rich in anhydride or carboxyl.
Through the technical scheme, compared with the prior art, the invention has the following beneficial effects:
(1) the water-based alkyd acrylic hybrid resin is water-based and acrylic acid modified alkyd resin, does not contain a surfactant, is dispersed in water after being neutralized by carboxyl carried by the hybrid resin, and has excellent water resistance.
(2) According to the invention, hydrophilic fatty acid modified acrylic resin is introduced into the alkyd resin, so that the hardness, drying speed and water resistance of the water-based alkyd acrylic hybrid resin are improved.
(3) The alkyd acrylic hybrid resin of the invention introduces chemical covalent bonds which have high bond energy and are difficult to break, such as carbon-carbon bonds, carbon-oxygen bonds and the like, on the molecular structure, thereby improving the heat storage capacity of the hybrid resin.
(4) The water-based alkyd acrylic hybrid resin disclosed by the invention combines excellent wettability of alkyd resin and acrylic acid and the bearing capacity of pigment and filler, can quickly wet and disperse the pigment and filler, and also has the quick wetting capacity on steel substrates. The gloss and the fullness of a paint film take the advantages of alkyd resin and acrylic resin into account, and when the color volume ratio is 1: at 1, 60 ℃ gloss can reach between 85 and 90.
(5) Coatings prepared from aqueous alkyd acrylic hybrid resins are suitable for use in the large-scale civil coatings and industrial coatings sectors, for example: steel structure coating, agricultural mechanical coating, metal mechanical part coating, woodenware coating, indoor water pipe coating and the like.
Drawings
FIG. 1 is a scanning electron microscope image of a waterborne alkyd acrylic hybrid resin of example 1 of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The invention provides a preparation method of a water-based alkyd acrylic hybrid resin, which comprises the following steps:
(1) the preparation of the basic alkyd resin, its raw material composition and formulation are shown in table 1.
The preparation method comprises the following steps: adding raw materials into a clean reaction kettle, heating to 180 ℃ in a nitrogen atmosphere, keeping the temperature for 1h, and collecting condensed water azeotroped with dimethylbenzene. And continuously heating to 225 ℃, keeping the temperature until the raw material becomes transparent and clear, continuously heating to 245 ℃ until the acid value of the alkyd resin is reduced to be less than 10mgKOH/g, cooling, diluting and discharging to obtain the basic alkyd resin.
TABLE 1 base alkyd resin raw Material composition and compounding ratio
(2) The raw material composition and the ratio of the fatty acid modified acrylic prepolymer are shown in table 2.
The preparation method comprises the following steps: dimethylbenzene accounting for 18 wt% of the total mass of the raw materials is used as a kettle bottom solvent, the raw materials are uniformly mixed, and then the mixture is dripped into a reaction kettle at the temperature of 140 ℃, wherein the dripping time is 6 hours. After the dropwise addition, reacting at the constant temperature of 140 ℃ for 2h, cooling and discharging to obtain the fatty acid modified acrylic prepolymer.
TABLE 2 raw material composition and compounding ratio of fatty acid-modified acrylic prepolymer
(3) The raw material composition and the mixture ratio of the preparation of the water-based alkyd acrylic hybrid resin are shown in table 3.
The preparation method comprises the following steps: and (2) putting the fatty acid modified acrylic prepolymer and the basic alkyd resin into a reaction kettle, mixing, heating to 180 ℃ in a nitrogen atmosphere for esterification, ending the reaction when the acid value is 25mgKOH/g, cooling to 120 ℃, adding ethylene glycol monobutyl ether, continuously cooling to 80 ℃, adding triethylamine, and then adding water for dilution until the solid mass is 45%, thereby obtaining the water-based alkyd acrylic hybrid resin.
TABLE 3 raw material composition and compounding ratio of water-based alkyd acrylic hybrid resin
As can be seen from FIG. 1, the waterborne alkyd acrylic hybrid resin prepared by the invention is in a porous cotton-like floccule, which shows that the fatty acid modified acrylic prepolymer is completely connected to the molecular structure of the alkyd resin through chemical bonds, and the fatty acid modified acrylic prepolymer and the alkyd resin form a homogeneous system. In addition, white gaps in fig. 1 are light-transmitting positions of a scanning electron microscope, which verifies that the waterborne alkyd acrylic hybrid resin has an obvious cavity inside, and a porous structure can enable oxygen to penetrate more deeply, so that the resin has a faster drying speed, a higher crosslinking density and a more compact three-dimensional network structure, and a coating prepared from the hybrid resin has better water resistance.
Example 2
The invention provides a preparation method of a water-based alkyd acrylic hybrid resin, which comprises the following steps:
(1) the base alkyd resin was prepared according to the same method as in example 1.
(2) The raw material composition and the ratio of the fatty acid modified acrylic prepolymer are shown in table 4.
The preparation method comprises the following steps: dimethylbenzene accounting for 18 wt% of the total mass of the raw materials is used as a kettle bottom solvent, the raw materials are uniformly mixed, and then the mixture is dripped into a reaction kettle at the temperature of 140 ℃, wherein the dripping time is 6 hours. After the dropwise addition, reacting at the constant temperature of 140 ℃ for 2h, cooling and discharging to obtain the fatty acid modified acrylic prepolymer.
TABLE 4 raw material composition and compounding ratio of fatty acid-modified acrylic prepolymer
(3) The raw material composition and the mixture ratio of the preparation of the water-based alkyd acrylic hybrid resin are shown in table 5.
The preparation method comprises the following steps: and (2) putting the fatty acid modified acrylic prepolymer and the basic alkyd resin into a reaction kettle, mixing, heating to 180 ℃ in a nitrogen atmosphere for esterification, ending the reaction when the acid value is 25mgKOH/g, cooling to 120 ℃, adding ethylene glycol monobutyl ether, continuously cooling to 80 ℃, adding dimethylethanolamine, and then adding water for dilution until the solid mass is 40%, thereby obtaining the water-based alkyd acrylic hybrid resin.
TABLE 5 raw material composition and compounding ratio of water-based alkyd acrylic hybrid resin
Example 3
The invention provides a preparation method of a water-based alkyd acrylic hybrid resin, which comprises the following steps:
(1) the preparation of the basic alkyd resin, its raw material composition and formulation are shown in table 6.
The preparation method comprises the following steps: adding raw materials into a clean reaction kettle, heating to 180 ℃ in a nitrogen atmosphere, keeping the temperature for 1h, and collecting condensed water azeotroped with dimethylbenzene. And continuously heating to 225 ℃, keeping the temperature until the raw material becomes transparent and clear, continuously heating to 245 ℃ until the acid value of the alkyd resin is reduced to be less than 10mgKOH/g, cooling, diluting and discharging to obtain the basic alkyd resin polymer.
TABLE 6 composition of basic alkyd resin raw materials and proportions
(2) The raw material composition and the compounding ratio of the fatty acid-modified acrylic prepolymer are shown in table 7.
The preparation method comprises the following steps: dimethylbenzene accounting for 18 wt% of the total mass of the raw materials is used as a kettle bottom solvent, the raw materials are uniformly mixed, and then the mixture is dripped into a reaction kettle at the temperature of 140 ℃, wherein the dripping time is 6 hours. After the dropwise addition, reacting at the constant temperature of 140 ℃ for 2h, cooling and discharging to obtain the fatty acid modified acrylic prepolymer.
TABLE 7 raw material composition and compounding ratio of fatty acid-modified acrylic prepolymer
(3) The raw material composition and the mixture ratio of the preparation of the waterborne alkyd acrylic hybrid resin are shown in table 8.
The preparation method comprises the following steps: and (2) putting the fatty acid modified acrylic prepolymer and the basic alkyd resin into a reaction kettle, mixing, heating to 180 ℃ in a nitrogen atmosphere for esterification, ending the reaction when the acid value is 25mgKOH/g, cooling to 120 ℃, adding ethylene glycol monobutyl ether, continuously cooling to 80 ℃, adding triethylamine, and then adding water for dilution until the solid mass is 50%, thereby obtaining the water-based alkyd acrylic hybrid resin.
TABLE 8 raw material composition and compounding ratio of water-based alkyd acrylic hybrid resin
Example 4
The preparation method of the water-based alkyd acrylic paint by using the water-based alkyd acrylic hybrid resin comprises the following steps:
respectively adding the water-based alkyd acrylic hybrid resin prepared in the embodiments 1-3 of the invention, a drier, butyl glycol ether, isopropanol and water into a paint mixing tank, dispersing the resin at a rotation speed of 400-800r/min, sequentially adding the prepared 75% titanium white slurry into the paint mixing tank, increasing the rotation speed to 800-1000r/min for high-speed dispersion, continuously adding a wetting agent, a leveling agent and a defoaming agent into the paint mixing tank at the rotation speed, and adding water for dilution until the paint viscosity reaches 30-40s in 4 cups after the fineness reaches 10 mu m, thereby obtaining the water-based alkyd acrylic paint. The results of the performance test of this coating are shown in Table 9.
TABLE 9 test results of the properties of the coating of the present invention
As can be seen from Table 9, after the waterborne alkyd acrylic hybrid resin is prepared into a coating, the water resistance is excellent, and the immersion time in water can reach more than 30 d. The water-based alkyd acrylic hybrid resin can be dried within 6.5h in terms of drying rate, has the characteristic of high gloss, and has better decorative effect compared with the commercially available alkyd resin.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. The water-based alkyd acrylic hybrid resin is characterized by comprising the following raw materials in parts by weight:
15-35 parts of fatty acid modified acrylic prepolymer, 15-35 parts of basic alkyd resin, 1-12 parts of solvent, 1-5 parts of neutralizer and 35-55 parts of water;
the fatty acid modified acrylic prepolymer is prepared from the following raw materials in parts by weight: 1-50 parts of fatty acid, 1-99 parts of (methyl) acrylic acid and ester monomers thereof, 1-50 parts of vinyl monomers, 1-15 parts of double-bond-containing anhydride or dibasic acid, 10-30 parts of solvent and 0.5-5 parts of initiator;
the basic alkyd resin is prepared from the following raw materials in parts by weight: 30-70 parts of fatty acid, 10-40 parts of polybasic acid, 10-40 parts of polyalcohol, 1-15 parts of monobasic acid, 0.1-1 part of antioxidant, 0.1-1 part of catalyst and 2-10 parts of solvent;
the solvent is one or more of ethylene glycol butyl ether, propylene glycol methyl ether, propylene glycol butyl ether, xylene, S100 solvent, n-butanol and isopropanol;
the neutralizing agent is one or more of triethylamine, ammonia water and dimethylethanolamine.
2. The waterborne alkyd acrylic hybrid resin of claim 1, wherein the fatty acid is one or more of linolenic acid, linoleic acid, eleostearic acid, soya-oleic acid, tall oil fatty acid, and oleic acid.
3. The waterborne alkyd acrylic hybrid resin of claim 1, the (methyl) acrylic acid and the ester monomer thereof are one or more of isooctyl acrylate, acrylic acid, isobornyl acrylate, n-butyl acrylate, methyl acrylate, ethyl acrylate, n-octyl acrylate, ethoxyethoxyethoxyethyl acrylate, 2-hydroxyethyl acrylate, 2-hydroxypropyl acrylate, methyl methacrylate, methacrylic acid, isobutyl methacrylate, octadecyl methacrylate, acetoacetoxy methacrylate, glycidyl methacrylate, isooctyl methacrylate, gamma-methacryloxypropyltriisopropoxysilane, gamma-methacryloxypropyltrimethoxysilane, gamma-methacryloxypropyltriethoxysilane and lauryl methacrylate.
4. The waterborne alkyd acrylic hybrid resin of claim 1, wherein the vinyl monomer is one or more of styrene, alpha-methylstyrene, vinyltrimethoxysilane, vinyltriethoxysilane, and vinyltriisopropoxysilane.
5. The waterborne alkyd acrylic hybrid resin of claim 1, wherein the double bond containing anhydride or diacid is one or more of maleic anhydride, tetrahydrophthalic anhydride, maleic acid, fumaric acid, and itaconic acid.
6. The waterborne alkyd acrylic hybrid resin of claim 1, wherein the initiator is t-butyl peroxybenzoate or di-t-amyl peroxide.
7. The waterborne alkyd acrylic hybrid resin of claim 1, wherein the polybasic acid is one or more of phthalic anhydride, isophthalic acid, terephthalic acid, tetrahydrophthalic anhydride, and adipic acid;
the polyalcohol is one or more of glycerol, trimethylolpropane, ethylene glycol, neopentyl glycol and pentaerythritol;
the monoacid is benzoic acid.
8. The waterborne alkyd acrylic hybrid resin of claim 1, wherein the antioxidant is triphenyl phosphite or hypophosphorous acid;
the catalyst is titanate or triphenylphosphine.
9. The preparation method of the water-based alkyd acrylic hybrid resin as claimed in any one of claims 1 to 8, comprising the following steps:
mixing the fatty acid modified acrylic prepolymer and the basic alkyd resin, heating to the temperature of 175-185 ℃ for esterification reaction, ending the reaction when the acid value is 20-50mgKOH/g, cooling to the temperature of 110-120 ℃, adding the solvent, continuously cooling to the temperature of 70-80 ℃, adding the neutralizing agent, and then adding water for dilution to obtain the water-based alkyd acrylic hybrid resin; wherein the mass of the solid of the water-based alkyd acrylic hybrid resin is 30-50%.
10. The preparation method of the water-based alkyd acrylic hybrid resin according to claim 9, wherein the fatty acid modified acrylic prepolymer is prepared by the following steps:
mixing fatty acid, (methyl) acrylic acid and ester monomers thereof, vinyl monomers, double-bond-containing acid anhydride or dibasic acid and an initiator, dripping the mixture into a solvent in multiple steps, and reacting at constant temperature for 1-3 hours after finishing dripping to obtain a fatty acid modified acrylic prepolymer;
wherein the dropping time is 3-9h, and the temperature in the dropping process is 110-150 ℃.
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Application publication date: 20210625 |