CN108517164B - Low-gloss acrylic resin for extinction electrophoresis coating and preparation method thereof - Google Patents
Low-gloss acrylic resin for extinction electrophoresis coating and preparation method thereof Download PDFInfo
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- CN108517164B CN108517164B CN201810217013.2A CN201810217013A CN108517164B CN 108517164 B CN108517164 B CN 108517164B CN 201810217013 A CN201810217013 A CN 201810217013A CN 108517164 B CN108517164 B CN 108517164B
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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
- C09D5/44—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes for electrophoretic applications
- C09D5/4407—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes for electrophoretic applications with polymers obtained by polymerisation reactions involving only carbon-to-carbon unsaturated bonds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/02—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polycarbonates or saturated polyesters
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Abstract
The invention relates to a preparation method of low-gloss acrylic resin for a photoelectric electrophoretic coating, which is prepared from the following raw materials in parts by mass: 3-4 parts of isooctyl methacrylate, 6-9 parts of n-butyl acrylate, 5-8 parts of methyl methacrylate, 1-3 parts of styrene, 0.5-1 part of acrylic acid, 1-2 parts of 2-hydroxyethyl methacrylate, 3-4 parts of 2-hydroxyethyl acrylate, 3-4 parts of 2-hydroxypropyl acrylate, 2-6 parts of polycarbonate, 0.05-0.3 part of dinonylnaphthalenesulfonic acid, 0.08-0.2 part of composite initiator, 1-2 parts of neutralizer, 0.01-0.02 part of defoaming agent, 8-15 parts of n-butanol, 8-15 parts of isopropanol and 10-50 parts of deionized water. The finally prepared electrophoretic paint has good extinction effect (the detection of a 60-degree gloss meter is less than 10 degrees), can be stored for more than one year, has no layering phenomenon and has good stability; and the paint film has good flatness and strong pollution resistance.
Description
Technical Field
The invention relates to a low-gloss acrylic resin for a photoelectric electrophoretic coating and a preparation method thereof, belonging to the technical field of coatings.
Background
Electrophoresis is one of the most effective methods for coating metal workpieces. The electrophoretic coating is a novel coating with low pollution, energy conservation, resource conservation and good corrosion resistance, has the advantages of smooth coating and good water resistance and chemical resistance, is easy to realize mechanization and automation of the coating industry, is suitable for coating workpieces with edges, corners and holes, has complex shapes, and is widely applied to coating hardware such as automobiles, automatic vehicles, electromechanics, household appliances and the like.
With the continuous development of the electrophoretic coating, the electrophoretic coating has more and more market applications, and has higher and higher requirements on the glossiness, the stability and the like of the electrophoretic coating. After the existing electrophoretic coating is added with the flatting agent, the glossiness of the electrophoretic coating can reach low light (the glossiness measured by a 60-degree gloss meter is less than or equal to 10 degrees), but the stability of the electrophoretic coating is poor, the electrophoretic coating can be layered after being stored for 3-5 months, and a paint film is uneven and not fine after being used. Development of a novel low-gloss acrylic resin for a high-stability photovoltaic electrophoretic paint has been a research direction.
Disclosure of Invention
The invention aims to solve the technical problem of providing a low-gloss acrylic resin for a high-stability extinction electrophoresis coating and a preparation method thereof aiming at the prior art.
The technical scheme adopted by the invention for solving the problems is as follows: the low-gloss acrylic resin for the extinction electrophoresis coating is prepared from the following raw materials in parts by mass: 3-4 parts of isooctyl methacrylate, 6-9 parts of n-butyl acrylate, 5-8 parts of methyl methacrylate, 1-3 parts of styrene, 0.5-1 part of acrylic acid, 1-2 parts of 2-hydroxyethyl methacrylate, 3-4 parts of 2-hydroxyethyl acrylate, 3-4 parts of 2-hydroxypropyl acrylate, 2-6 parts of polycarbonate, 0.05-0.3 part of dinonylnaphthalenesulfonic acid, 0.08-0.2 part of composite initiator, 1-2 parts of neutralizer, 0.01-0.02 part of defoaming agent, 8-15 parts of n-butanol, 8-15 parts of isopropanol and 10-50 parts of deionized water.
The number average molecular weight of the polycarbonate is 2 to 10 ten thousand.
The composite initiator is prepared by compounding azodiisobutyronitrile and DCP (dicumyl peroxide) according to the mass ratio of 1: 2-5. DCP is adopted as an initiator, so that side chain reaction can be increased, the adhesive force and the corrosion resistance of the coating are increased, and particularly the anti-deformability is obviously enhanced; the adoption of the azodiisobutyronitrile can promote the conversion rate of the monomer, and the compatibility of the azodiisobutyronitrile and the monomer realizes low-temperature initiation and high-temperature continuous reaction. As heat energy is released in the reaction process, the temperature of the system rises and generates larger fluctuation, and in order to ensure that the reaction is not influenced by temperature change, the introduced DCP initiator mainly ensures stable reaction at high temperature and ensures high-low temperature uniform reaction.
The neutralizer is triethanolamine, methyldiethanolamine or triethylamine.
The preparation method of the low-gloss acrylic resin for the extinction electrophoresis coating comprises the following steps:
step one, preparing a mixed solution
Mixing isooctyl methacrylate, n-butyl acrylate, methyl methacrylate, styrene, acrylic acid, 2-hydroxyethyl methacrylate, 2-hydroxyethyl acrylate, 2-hydroxypropyl acrylate, polycarbonate and dinonyl naphthalene sulfonic acid to form a mixed solution;
step two, forming water-soluble acrylic resin
Heating the reaction container to 95-105 ℃ by using n-butyl alcohol, isopropanol and deionized water accounting for 5-15% of the total amount of the deionized water as bottom materials, dropwise adding the mixed solution prepared in the first step into the reaction container, wherein the dropwise adding time is 150-200min, dropwise adding a composite initiator, dropwise adding the composite initiator for four times, and controlling the dropwise adding speed according to the intensity of the reaction; and then preserving the temperature of the reaction vessel for 150-280min, cooling the reaction vessel to below 60 ℃, adding a neutralizing agent into the reaction vessel, uniformly stirring, adding a defoaming agent into the reaction vessel, and finally adding the rest deionized water for dilution and molding.
Compared with the prior art, the invention has the advantages that:
the invention adopts dinonyl naphthalenesulfonic acid for dewatering, adds polycarbonate as a flatting agent, adopts polycarbonate with the molecular weight of 2-10 ten thousand, improves the using amount of the polycarbonate, increases the using amount of the hydroxyl monomer, reduces the using amount of acrylic acid and an initiator, ensures that the finally prepared electrophoretic paint has good flatting effect (the using amount of a 60-degree gloss instrument is less than 10 degrees), has no layering phenomenon after being stored for more than one year and has good stability; and the paint film has good flatness and strong pollution resistance. In the reaction process, the compound initiator is dripped for four times, the reaction is complete, and the method is safe and controllable.
Detailed Description
The present invention will be described in further detail with reference to examples.
The invention relates to a low-gloss acrylic resin for a photoelectric electrophoretic coating, which is prepared from the following raw materials in parts by weight: 3-4 parts of isooctyl methacrylate, 6-9 parts of n-butyl acrylate, 5-8 parts of methyl methacrylate, 1-3 parts of styrene, 0.5-1 part of acrylic acid, 1-2 parts of 2-hydroxyethyl methacrylate, 3-4 parts of 2-hydroxyethyl acrylate, 3-4 parts of 2-hydroxypropyl acrylate, 2-6 parts of polycarbonate, 0.05-0.3 part of dinonylnaphthalenesulfonic acid, 0.08-0.2 part of composite initiator, 1-2 parts of neutralizer, 0.01-0.02 part of defoaming agent, 8-15 parts of n-butanol, 8-15 parts of isopropanol and 10-50 parts of deionized water.
The number average molecular weight of the polycarbonate is 2-10 ten thousand;
the composite initiator is azodiisobutyronitrile and DCP (dicumyl peroxide) which are compounded according to the mass ratio of 1:2-5, and the neutralizer is triethanolamine, methyldiethanolamine or triethylamine.
The preparation method of the low-gloss acrylic resin for the extinction electrophoresis coating comprises the following steps:
step one, preparing a mixed solution
Mixing isooctyl methacrylate, n-butyl acrylate, methyl methacrylate, styrene, acrylic acid, 2-hydroxyethyl methacrylate, 2-hydroxyethyl acrylate, 2-hydroxypropyl acrylate, polycarbonate and dinonyl naphthalene sulfonic acid to form a mixed solution;
step two, forming water-soluble acrylic resin
Heating the reaction container to 95-105 ℃ by using n-butyl alcohol, isopropanol and deionized water accounting for 5-15% of the total amount of the deionized water as bottom materials, dropwise adding the mixed solution prepared in the first step into the reaction container, wherein the dropwise adding time is 150-200min, dropwise adding a composite initiator, dropwise adding the composite initiator for four times, and controlling the dropwise adding speed according to the intensity of the reaction; and then preserving the temperature of the reaction vessel for 150-280min, cooling the reaction vessel to below 60 ℃, adding a neutralizing agent into the reaction vessel, uniformly stirring, adding a defoaming agent into the reaction vessel, and finally adding the rest deionized water for dilution and molding.
The raw material components of the embodiments 1-5 of the invention are as follows:
example 1, a low gloss acrylic resin for a photovoltaic coating, which is prepared from the following raw materials in percentage by mass: 3 parts of isooctyl methacrylate, 8 parts of n-butyl acrylate, 7 parts of methyl methacrylate, 2 parts of styrene, 0.5 part of acrylic acid, 2 parts of 2-hydroxyethyl methacrylate, 3 parts of 2-hydroxyethyl acrylate, 3 parts of 2-hydroxypropyl acrylate, 6 parts of polycarbonate (the number average molecular weight is 7 ten thousand), 0.1 part of dinonylnaphthalenesulfonic acid, 0.1 part of composite initiator (azodiisobutyronitrile and DCP (dicumyl peroxide) are in a ratio of 1: 3), 1 part of triethanolamine neutralizer, 0.01 part of defoaming agent, 10 parts of n-butanol, 10 parts of isopropanol and 30 parts of deionized water.
Example 2, a low gloss acrylic resin for a photovoltaic coating, which is prepared from the following raw materials in percentage by mass: 4 parts of isooctyl methacrylate, 8 parts of n-butyl acrylate, 6 parts of methyl methacrylate, 3 parts of styrene, 1 part of acrylic acid, 1.5 parts of 2-hydroxyethyl methacrylate, 3.5 parts of 2-hydroxyethyl acrylate, 3.5 parts of 2-hydroxypropyl acrylate, 5 parts of polycarbonate (the number average molecular weight is 6 ten thousand), 0.15 part of dinonylnaphthalenesulfonic acid, 0.08 part of a composite initiator (azodiisobutyronitrile and DCP (dicumyl peroxide) are in a ratio of 1: 3), 1.2 parts of a triethanolamine neutralizer, 0.01 part of a defoaming agent, 10 parts of n-butanol, 10 parts of isopropanol and 30 parts of deionized water.
Example 3, a low gloss acrylic resin for a photovoltaic coating, which is prepared from the following raw materials in percentage by mass: 3.5 parts of isooctyl methacrylate, 9 parts of n-butyl acrylate, 8 parts of methyl methacrylate, 2 parts of styrene, 0.8 part of acrylic acid, 1 part of 2-hydroxyethyl methacrylate, 4 parts of 2-hydroxyethyl acrylate, 3 parts of 2-hydroxypropyl acrylate, 4 parts of polycarbonate (the number average molecular weight is 8 ten thousand), 0.05 part of dinonylnaphthalenesulfonic acid, 0.1 part of composite initiator (azodiisobutyronitrile and DCP (dicumyl peroxide) are in a ratio of 1: 2), 1.5 parts of methyldiethanolamine neutralizer, 0.02 part of antifoaming agent, 15 parts of n-butanol, 15 parts of isopropanol and 40 parts of deionized water.
Example 4, a low gloss acrylic resin for a photovoltaic electrophoretic coating, which is prepared from the following raw materials in parts by mass: 4 parts of isooctyl methacrylate, 6 parts of n-butyl acrylate, 8 parts of methyl methacrylate, 3 parts of styrene, 1 part of acrylic acid, 2-hydroxyethyl methacrylate, 3 parts of 2-hydroxyethyl acrylate, 3 parts of 2-hydroxypropyl acrylate, 4 parts of polycarbonate (the number average molecular weight is 8 ten thousand), 0.2 part of dinonylnaphthalenesulfonic acid, 0.2 part of composite initiator (azodiisobutyronitrile and DCP (dicumyl peroxide) are in a ratio of 1: 5), 1.5 parts of methyldiethanolamine neutralizer, 0.02 part of defoaming agent, 10 parts of n-butanol, 8 parts of isopropanol and 20 parts of deionized water.
Example 5, a low gloss acrylic resin for a photovoltaic electrophoretic coating, which is prepared from the following raw materials in percentage by mass: 3.5 parts of isooctyl methacrylate, 9 parts of n-butyl acrylate, 5 parts of methyl methacrylate, 1 part of styrene, 0.5 part of acrylic acid, 1 part of 2-hydroxyethyl methacrylate, 4 parts of 2-hydroxyethyl acrylate, 4 parts of 2-hydroxypropyl acrylate, 3 parts of polycarbonate (the number average molecular weight is 8 ten thousand), 0.2 part of dinonylnaphthalenesulfonic acid, 0.2 part of composite initiator (azodiisobutyronitrile and DCP (dicumyl peroxide) are in a ratio of 1: 4), 1.5 parts of methyldiethanolamine neutralizer, 0.02 part of antifoaming agent, 10 parts of n-butanol, 8 parts of isopropanol and 20 parts of deionized water.
The comparative examples of the water-soluble acrylic resin comprise the following raw material components:
comparative example 1, an acrylic resin for an electrodeposition coating, prepared from the following raw materials in parts by mass: 3 parts of isooctyl methacrylate, 8 parts of n-butyl acrylate, 7 parts of methyl methacrylate, 2 parts of styrene, 0.5 part of acrylic acid, 2 parts of 2-hydroxyethyl methacrylate, 3 parts of 2-hydroxyethyl acrylate, 3 parts of 2-hydroxypropyl acrylate, 6 parts of polycarbonate (the number average molecular weight is 7 ten thousand), 0.1 part of composite initiator (azodiisobutyronitrile and DCP (dicumyl peroxide) are in a ratio of 1: 3), 1 part of triethanolamine neutralizer, 0.01 part of defoaming agent, 10 parts of n-butanol, 10 parts of isopropanol and 30 parts of deionized water.
Namely, it is different from example 1 only in that comparative example 1 does not use dinonylnaphthalenesulfonic acid.
Comparative example 2, an acrylic resin for an electrodeposition coating, which was prepared from the following raw materials in mass fraction: 3 parts of isooctyl methacrylate, 8 parts of n-butyl acrylate, 7 parts of methyl methacrylate, 2 parts of styrene, 0.5 part of acrylic acid, 3 parts of 2-hydroxyethyl methacrylate, 6 parts of polycarbonate (the number average molecular weight is 7 ten thousand), 0.1 part of dinonyl naphthalene sulfonic acid, 0.1 part of a composite initiator (azodiisobutyronitrile and DCP (dicumyl peroxide) are in a ratio of 1: 3), 1 part of triethanolamine neutralizer, 0.01 part of defoaming agent, 10 parts of n-butanol, 10 parts of isopropanol and 30 parts of deionized water.
I.e., differs from example 1 only in that only 2-hydroxyethyl methacrylate is used, and no 2-hydroxyethyl acrylate and no 2-hydroxypropyl acrylate are used (i.e., only 2-hydroxyethyl methacrylate alone provides the hydroxyl functionality).
Comparative example 3
It differs from example 1 only in that silicon dioxide is used as matting agent.
Comparative example 4
It differs from example 1 only in that the number average molecular weight of the polycarbonate is 5000.
Comparative example 5
The acrylic resin for the electrophoretic coating is prepared from the following raw materials in percentage by mass: 3 parts of isooctyl methacrylate, 8 parts of n-butyl acrylate, 7 parts of methyl methacrylate, 2 parts of styrene, 3 parts of acrylic acid, 6 parts of 2-hydroxyethyl methacrylate, 6 parts of polycarbonate (the number average molecular weight is 7 ten thousand), 0.1 part of dinonyl naphthalene sulfonic acid, 1 part of a composite initiator (azodiisobutyronitrile and DCP (dicumyl peroxide) in a ratio of 1: 3), 1 part of triethanolamine neutralizer, 0.01 part of defoaming agent, 10 parts of n-butyl alcohol, 10 parts of isopropanol and 30 parts of deionized water.
It differs from example 1 only in that: the amount of acrylic acid and the composite initiator is significantly increased.
The gloss and stability measurements of examples 1-5 and comparative examples 1-5 are shown in Table 1.
And (3) gloss detection: after the coating prepared by the same method is formed into a film, the film is detected by a 60-degree gloss meter.
Stability: storing at normal temperature.
TABLE 1
| Degree of gloss | Appearance of film formation | Resin stability | |
| Example 1 | 6 degree | The paint film is smooth and fine | Can be stored at normal temperature for one year without layering |
| Example 2 | 7 degree | The paint film is smooth and fine | Can be stored at normal temperature for one year without layering |
| Example 3 | 9 degree | The paint film is smooth and fine | Can be stored at normal temperature for one year without layering |
| Example 4 | 8 degree | The paint film is smooth and fine | Can be stored at normal temperature for one year without layering |
| Example 5 | 9 degree | The paint film is smooth and fine | Can be stored at normal temperature for one year without layering |
| Comparative example 1 | 35 degree | Uneven and rough paint film | Storing at room temperature for 6 months, and demixing |
| Comparative example 2 | 28 degree | To generate spots | Storing at room temperature for 3 months, and demixing |
| Comparative example 3 | 8 degree | The paint film is uneven and rough | Storing at room temperature for 3 months, and demixing |
| Comparative example 4 | 35 degree | Film leveling | Can be stored at normal temperature for one year without layering |
| Comparative example 5 | 19 degree | Film leveling | Can be stored at normal temperature for one year without layering |
In addition to the above embodiments, the present invention also includes other embodiments, and any technical solutions formed by equivalent transformation or equivalent replacement should fall within the scope of the claims of the present invention.
Claims (4)
1. A low-gloss acrylic resin for a photoelectric electrophoretic coating is characterized in that: the material is prepared from the following raw materials in parts by mass: 3-4 parts of isooctyl methacrylate, 6-9 parts of n-butyl acrylate, 5-8 parts of methyl methacrylate, 1-3 parts of styrene, 0.5-1 part of acrylic acid, 1-2 parts of 2-hydroxyethyl methacrylate, 3-4 parts of 2-hydroxyethyl acrylate, 3-4 parts of 2-hydroxypropyl acrylate, 2-6 parts of polycarbonate, 0.05-0.3 part of dinonylnaphthalenesulfonic acid, 0.08-0.2 part of composite initiator, 1-2 parts of neutralizer, 0.01-0.02 part of defoaming agent, 8-15 parts of n-butanol, 8-15 parts of isopropanol and 10-50 parts of deionized water;
the number average molecular weight of the polycarbonate is 2-10 ten thousand, and the composite initiator is formed by compounding azodiisobutyronitrile and DCP according to the mass ratio of 1: 2-5.
2. The low gloss acrylic resin for an electroless electrophoretic paint according to claim 1, wherein: the neutralizing agent is triethanolamine, methyldiethanolamine or triethylamine.
3. A method for producing a low-gloss acrylic resin for an electroless electrophoretic paint according to claim 1, characterized in that:
step one, preparing a mixed solution
Mixing isooctyl methacrylate, n-butyl acrylate, methyl methacrylate, styrene, acrylic acid, 2-hydroxyethyl methacrylate, 2-hydroxyethyl acrylate, 2-hydroxypropyl acrylate, polycarbonate and dinonyl naphthalene sulfonic acid to form a mixed solution;
step two, forming water-soluble acrylic resin
Heating the reaction container to 95-105 ℃ by using n-butyl alcohol, isopropanol and deionized water accounting for 5-15% of the total amount of the deionized water as bottom materials, dropwise adding the mixed solution prepared in the first step into the reaction container for 200min at 150-; and then preserving the temperature of the reaction vessel for 150-280min, cooling the reaction vessel to below 60 ℃, adding a neutralizing agent into the reaction vessel, uniformly stirring, adding a defoaming agent into the reaction vessel, and finally adding the rest deionized water for dilution and molding.
4. The method for producing a low-gloss acrylic resin for an electroless electrophoretic paint according to claim 3, comprising: the composite initiator is dripped for four times, and the dripping speed is controlled according to the reaction intensity.
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| JP2835481B2 (en) * | 1993-05-28 | 1998-12-14 | ハニー化成株式会社 | Matte anion resin composition for electrodeposition coating |
| CN102115526B (en) * | 2011-01-04 | 2012-11-28 | 中科院广州化学有限公司 | Extinction acrylic resin for anodic electrophoresis and preparation method thereof |
| CN102702411B (en) * | 2012-05-22 | 2014-12-03 | 东莞市英科水墨有限公司 | Core-shell matte emulsion as well as preparation method and application of core-shell matte emulsion in water matte gloss oil |
| CN105859954B (en) * | 2016-05-05 | 2018-03-13 | 常熟林润氟硅材料有限公司 | A kind of preparation method of water-based matt acrylic emulsion |
| CN105968253B (en) * | 2016-06-01 | 2018-02-02 | 嘉宝莉化工集团股份有限公司 | It is a kind of water-based from mat acrylic emulsion and preparation method and application |
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