CN111138599A - Preparation method of weather-resistant real stone paint emulsion - Google Patents
Preparation method of weather-resistant real stone paint emulsion Download PDFInfo
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- CN111138599A CN111138599A CN202010078824.6A CN202010078824A CN111138599A CN 111138599 A CN111138599 A CN 111138599A CN 202010078824 A CN202010078824 A CN 202010078824A CN 111138599 A CN111138599 A CN 111138599A
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- real stone
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- stone paint
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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
- C08F265/00—Macromolecular compounds obtained by polymerising monomers on to polymers of unsaturated monocarboxylic acids or derivatives thereof as defined in group C08F20/00
- C08F265/10—Macromolecular compounds obtained by polymerising monomers on to polymers of unsaturated monocarboxylic acids or derivatives thereof as defined in group C08F20/00 on to polymers of amides or imides
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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
- C08F265/00—Macromolecular compounds obtained by polymerising monomers on to polymers of unsaturated monocarboxylic acids or derivatives thereof as defined in group C08F20/00
- C08F265/04—Macromolecular compounds obtained by polymerising monomers on to polymers of unsaturated monocarboxylic acids or derivatives thereof as defined in group C08F20/00 on to polymers of esters
- C08F265/06—Polymerisation of acrylate or methacrylate esters on to polymers thereof
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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
- C09D151/00—Coating compositions based on graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Coating compositions based on derivatives of such polymers
- C09D151/003—Coating compositions based on graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Coating compositions based on derivatives of such polymers grafted on to macromolecular compounds obtained by reactions only involving unsaturated carbon-to-carbon bonds
-
- 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
- C09D5/1656—Antifouling paints; Underwater paints characterised by the film-forming substance
- C09D5/1662—Synthetic film-forming substance
Abstract
The invention provides a preparation method of a weather-resistant real stone paint emulsion, which comprises the following raw materials of water, an emulsifier, methyl methacrylate, isobutyl (meth) acrylate, methacrylamide, acrylic acid, an initiator, an oxidant, a reducing agent and the like. The emulsion is prepared by copolymerizing isobutyl (meth) acrylate and methyl methacrylate through a core-shell method, an inner core is formed by utilizing a seed emulsion, an outer core is formed by crosslinking and copolymerizing methyl methacrylate and part of isobutyl (meth) acrylate, and an outer protective layer is formed by self-crosslinking isobutyl acrylate. The novel real stone paint emulsion has the characteristics of good weather resistance, water resistance, stable paint mixing performance and the like.
Description
Technical Field
The invention relates to the technical field of real stone paint emulsion, in particular to a preparation method of real stone paint emulsion with excellent weather resistance, which is formed by copolymerizing an isobutyl acrylate monomer and methyl methacrylate.
Background
The stone-like paint is a paint product prepared by mainly adopting high-performance polymer emulsion, adding natural or artificial dyed colored sand with various colors and various auxiliary agents. As a building exterior wall coating, the stone-like paint is used outdoors and is often subjected to tests of outdoor environmental conditions such as wind, rain, sunshine and the like, so that the stone-like paint is required to have good water resistance, weather resistance and corrosion resistance.
The technical problem to be solved urgently is to seek a stain-resistant and sun-resistant high-performance real stone paint emulsion. Unlike styrene, isobutyl acrylate, isobutyl methacrylate and methyl methacrylate are cracked under the irradiation of ultraviolet rays to generate a color change reaction, so that the emulsion prepared by copolymerizing the isobutyl acrylate, the isobutyl methacrylate and the methyl methacrylate has excellent weather resistance, and the both are monomers with strong hydrophobicity and form a compact network structure through copolymerization, so that the real stone paint prepared by the emulsion has excellent water resistance, stain resistance and strength.
Disclosure of Invention
The invention aims to solve the technical problems and provides a preparation method of a weather-resistant real stone paint emulsion.
The weather-resistant real stone paint emulsion comprises the following components in parts by mass:
acrylate ester: 510 to 692;
methyl methacrylate: 214-396;
hydroxyethyl methacrylate: 815;
acrylamide: 8-15;
alkyl carboxylic acid crosslinking monomer: 20-30;
silane coupling agent: 4-10;
initiator: 2-5;
emulsifier: 9-11;
oxidizing agent: 0.88 to 1.28;
reducing agent: 0.62 to 1.22;
water: 800-1200.
The preparation method of the weather-resistant real stone paint emulsion comprises the following steps:
s1: preparing a kettle bottom solution: adding water and an emulsifier into a reaction kettle with a stirrer, a condenser and a constant flow pump, stirring and heating, and heating until the temperature in the kettle reaches 83-88 ℃;
s2: preparing an inner core pre-emulsion: adding water and an emulsifier into a container with metering stirring, then stirring until the emulsifier is uniformly distributed in the water, sequentially adding methyl methacrylate, acrylic ester, acrylic acid, hydroxyethyl methacrylate, methacrylamide and an initiator, and stirring for 10-20 minutes to obtain a uniformly mixed solution for later use;
s3: preparing an outer-layer pre-emulsion: adding water and an emulsifier into a container with metering stirring, then stirring until the emulsifier is uniformly distributed in the water, adding acrylate, methacrylamide and a silane coupling agent, and stirring for 10-20 minutes to obtain a uniformly mixed solution for later use;
s4: after the temperature of the kettle bottom solution is raised to 83-88 ℃, adding 5% of kernel pre-emulsion and an initiator, preserving the temperature for 20-30 minutes, uniformly and quickly feeding the kernel pre-emulsion into the kettle bottom by using a constant flow pump after the heat preservation is finished, keeping the dripping time at 120 minutes, and controlling the reaction temperature in the kettle at 85-88 ℃. After the dripping is finished, keeping the temperature for 0.5 hour, after the heat preservation is finished, dripping the outer-layer pre-emulsion for 60 minutes, keeping the temperature constant, and keeping the temperature for 0.5 hour after the dripping is finished;
s5: and (3) post-treatment of the emulsion: after the heat preservation is finished, cooling to 60-65 ℃, then simultaneously dripping an oxidant and a reducing agent, and preserving the heat for 10-15 minutes after finishing dripping;
s6: and after the heat preservation is finished, cooling to 50 ℃, then adjusting the pH value to 7-8 by using ammonia water, stirring for 30 minutes, filtering and discharging to obtain the novel real stone paint emulsion.
Further, the acrylate is at least one selected from isobutyl methacrylate and isobutyl acrylate.
Further, the emulsifier is selected from at least one of ammonium vinylpolyoxyethylene alkyl thionate or disodium sulfosuccinate.
Further, the alkyl carboxylic acid crosslinking monomer is selected from at least one of acrylic acid, methacrylic acid and itaconic acid.
Further, the silane coupling agent is selected from at least one of vinyltrimethoxysilane and vinyltriethoxysilane.
Further, the initiator is selected from at least one of ammonium persulfate, sodium persulfate or potassium persulfate.
Further, the oxidizing agent is selected from a tert-butyl hydroperoxide solution with the mass fraction of 5%, and the reducing agent is selected from a sodium formaldehyde sulfoxylate solution with the mass fraction of 5%.
The invention has the following characteristics:
(1) the novel monomer isobutyl (meth) acrylate is adopted to form an inner core by utilizing a seed emulsion method, and then is copolymerized with methyl methacrylate to form an outer core, a long chain is connected through a branched chain to form a compact net structure, the hardness and the caking property of a paint film are effectively improved, then an outer protective layer is formed by self-crosslinking through isobutyl ester under the assistance of a crosslinking agent, an inner-middle-outer three-layer structure is formed, the seed emulsion of the inner core ensures that the emulsion has a small particle size and reaction stability, two monomers in a middle layer are copolymerized to serve as an emulsion main body, the emulsion is ensured to have high strength by virtue of the compact net structure, the emulsion is not easy to decompose, and the self-polymerization of an outer main monomer is realized due to the extremely high hydrophobicity, so that. The novel emulsion comprises raw material components such as deionized water, an emulsifier, methyl methacrylate, isobutyl acrylate, acrylamide, acrylic acid, kettle bottom solution, an initiator, a reaction initiator, an oxidant, a reducing agent and the like. The raw material components react to generate the real stone paint emulsion with small particle size and stable structure through the process of forming the internal and external nuclear shell layer emulsion.
(2) The introduction of isobutyl methacrylate and isobutyl acrylate leads the synthesized emulsion to be more complex and more stable in spatial structure due to the existence of methyl and methyl ester copolymerization with the same existence of dimethyl, thereby leading the paint film to have high strength, and simultaneously, the paint film is not easy to decompose and drop when being blown by the sun, and the weather-resistant type of the paint film is more prominent.
(3) The product adopts seed emulsion core-shell copolymerization to obtain emulsion with an inner-middle-outer three-layer structure, the seed emulsion of the inner core ensures that the emulsion has small particle size and stability, the two monomers of the middle layer are copolymerized to be used as an emulsion main body, the emulsion is ensured to have extremely high strength and difficult decomposition by virtue of a compact net structure, and the self-polymerization of the main monomer of the outer layer is realized due to extremely high hydrophobicity, so that a paint film has excellent water resistance and weather resistance. The stone-like paint prepared by the structure has excellent comprehensive performance and high stability, and particularly has an outstanding appearance on the weather-resistant type upper surface.
The specific implementation mode is as follows:
the present invention will be described in detail with reference to examples.
Example 1:
(1) firstly, adding 510 parts of deionized water and 3 parts of ammonium vinyl polyoxyethylene alkyl thioether into a reaction kettle with a stirrer, a condenser and a constant flow pump, stirring and heating, and heating until the temperature in the kettle reaches 85 ℃ to prepare a uniformly mixed kettle bottom solution for later use; (2) adding 306 parts of deionized water and 4 parts of vinyl polyoxyethylene alkyl ammonium thioether into a container with metering stirring, then stirring until an emulsifier is uniformly distributed in water, sequentially adding 214 parts of methyl methacrylate, 392 parts of isobutyl acrylate, 25 parts of acrylic acid, 9.22 parts of hydroxyethyl methacrylate, 4.22 parts of acrylamide and 2 parts of potassium persulfate, and stirring for 10 minutes to obtain a uniformly mixed core pre-emulsion solution for later use; (3) adding 154 parts of water and 2 parts of vinyl polyoxyethylene alkyl ammonium thioether into a container with metering stirring, then stirring until an emulsifier is uniformly distributed in the water, adding 300 parts of isobutyl acrylate, 5 parts of methacrylamide and 4.7 parts of vinyl trimethoxy silane, and stirring for 10-20 minutes to obtain a uniformly mixed outer-layer pre-emulsion solution for later use; (4) heating the kettle bottom solution, adding 5% of kernel pre-emulsion and 0.7 part of sodium persulfate after the kettle bottom solution is heated to 83 ℃, preserving the temperature for 30 minutes, uniformly feeding the kernel pre-emulsion into the kettle bottom by using a constant flow pump after the heat preservation is finished, keeping the dropping time at 120 minutes, and controlling the reaction temperature in the kettle at 86 ℃. After the dripping is finished, the heat preservation is carried out for 0.5 hour, after the heat preservation is finished, the outer-layer pre-emulsion is dripped, the dripping time is 60 minutes, the temperature is kept constant at 86 ℃, and the heat preservation is carried out for 0.5 hour after the dripping is finished; (5) after the heat preservation is finished, the temperature is reduced to 60 ℃, then 0.9 part of oxidant and 0.65 part of reducer are simultaneously dripped, and the heat preservation is carried out for 15 minutes after the dripping is finished. And after the heat preservation is finished, cooling to 50 ℃, then adjusting the pH value to 7 with ammonia water, stirring for 30 minutes, filtering and discharging to obtain the novel real stone paint emulsion.
Example 2
(1) Firstly, adding 510 parts of deionized water and 4 parts of ammonium vinyl polyoxyethylene alkyl thioether into a reaction kettle with a stirrer, a condenser and a constant flow pump, stirring and heating, and heating until the temperature in the kettle reaches 85 ℃ to prepare a uniformly mixed kettle bottom solution for later use; (2) adding 338 parts of deionized water and 4 parts of vinyl polyoxyethylene alkyl ammonium thioether into a container with metering stirring, then stirring until an emulsifier is uniformly distributed in water, sequentially adding 308 parts of methyl methacrylate, 299 parts of isobutyl acrylate, 22 parts of acrylic acid, 4.22 parts of hydroxyethyl methacrylate and 2 parts of potassium persulfate, and stirring for 15 minutes to obtain a uniformly mixed core pre-emulsion solution for later use; (3) adding 172 parts of water and 1 part of ammonium vinylpolyoxyethylene alkyl thioether into a container with metering stirring, then stirring until an emulsifier is uniformly distributed in the water, adding 299 parts of isobutyl acrylate, 5 parts of methacrylamide and 4.7 parts of vinyltrimethoxysilane, and stirring for 15 minutes to obtain a uniformly mixed outer-layer pre-emulsion solution for later use; the reaction, post-treatment and discharge of the subsequent experiment are all completed according to the process of the embodiment 1, so that the novel real stone paint emulsion can be obtained, and the novel real stone paint emulsion can be obtained.
Example 3
(1) Firstly, adding 656 parts of deionized water and 4 parts of ammonium vinyl polyoxyethylene alkyl thioether into a reaction kettle with a stirrer, a condenser and a constant flow pump, stirring and heating, and heating until the temperature in the kettle reaches 88 ℃ to prepare a uniformly mixed kettle bottom solution for later use; (2) adding 296 parts of deionized water and 4 parts of vinyl polyoxyethylene alkyl ammonium thioether into a container with metering stirring, then stirring until an emulsifier is uniformly distributed in water, sequentially adding 396 parts of methyl methacrylate, 255 parts of isobutyl acrylate, 25 parts of acrylic acid, 4.22 parts of hydroxyethyl methacrylate and 2 parts of potassium persulfate, and stirring for 20 minutes to obtain a uniformly mixed core pre-emulsion solution for later use; (3) adding 148 parts of water and 1 part of ammonium vinylpolyoxyethylene alkyl thioether into a container with metering stirring, then stirring until an emulsifier is uniformly distributed in the water, adding 255 parts of isobutyl acrylate, 5 parts of methacrylamide and 4.7 parts of vinyltrimethoxysilane, and stirring for 20 minutes to obtain a uniformly mixed outer-layer pre-emulsion solution for later use; the reaction, post-treatment and discharge of the subsequent experiment are all completed according to the process of the embodiment 1, so that the novel real stone paint emulsion can be obtained, and the novel real stone paint emulsion can be obtained.
Example 4
(1) Firstly, adding 510 parts of deionized water, 3.75 parts of ammonium vinyl polyoxyethylene alkyl thioether and 2 parts of disodium sulfosuccinate into a reaction kettle with a stirrer, a condenser and a constant flow pump, stirring and heating, and heating until the temperature in the kettle reaches 88 ℃ to prepare a uniformly mixed kettle bottom solution for later use; (2) adding 306 parts of deionized water and 4.25 parts of ammonium vinylpolyoxyethylene alkyl thioether into a container with metering stirring, then stirring until the emulsifier is uniformly distributed in water, adding 214 parts of methyl methacrylate, 342 parts of isobutyl acrylate, 25 parts of acrylic acid, 4.22 parts of hydroxyethyl methacrylate and 2 parts of potassium persulfate, and stirring for 18 minutes to obtain a uniformly mixed core pre-emulsion solution for later use; (3) adding 148 parts of water, 1 part of ammonium vinylpolyoxyethylene alkyl thioether and 0.5 part of disodium sulfosuccinate into a container with metering stirring, then stirring until an emulsifier is uniformly distributed in the water, adding 255 parts of isobutyl acrylate, 5 parts of methacrylamide and 10 parts of vinyl trimethoxy silane, and stirring for 20 minutes to obtain a uniformly mixed outer-layer pre-emulsion solution for later use; the reaction, post-treatment and discharge of the subsequent experiment are all completed according to the process of the embodiment 1, so that the novel real stone paint emulsion can be obtained, and the novel real stone paint emulsion can be obtained.
Comparative example 1
The synthesis was carried out according to the method described in patent CN 105255298A.
Comparative example 2
The synthesis was carried out according to the method described in patent CN 110452566A.
Comparative example 3
The product RS-8777 is prepared by Bardful and sold on the market as a comparative example.
And (3) performance detection:
performance testing was performed as described in the industry Standard JG/T24-2000.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.
The invention has the advantages that: the weather-resistant real stone paint emulsion disclosed by the invention has excellent weather resistance, and the adopted isobutyl acrylate, isobutyl methacrylate and methyl methacrylate are monomers with strong hydrophobicity, and form a dense net structure through copolymerization, so that the real stone paint prepared from the emulsion has excellent water resistance, stain resistance and strength.
Claims (8)
1. A weather-resistant real stone paint emulsion is characterized in that: the composite material comprises the following components in parts by mass:
acrylate ester: 510 to 692;
methyl methacrylate: 214-396;
hydroxyethyl methacrylate: 815;
acrylamide: 8-15;
alkyl carboxylic acid crosslinking monomer: 20-30;
silane coupling agent: 4-10;
initiator: 2-5;
emulsifier: 9-11;
oxidizing agent: 0.88 to 1.28;
reducing agent: 0.62 to 1.22;
water: 800-1200.
2. A preparation method of weather-resistant real stone paint emulsion is characterized by comprising the following steps: the method comprises the following steps:
s1: preparing a kettle bottom solution: adding water and an emulsifier into a reaction kettle with a stirrer, a condenser and a constant flow pump, stirring and heating, and heating until the temperature in the kettle reaches 83-88 ℃;
s2: preparing an inner core pre-emulsion: adding water and an emulsifier into a container with metering stirring, then stirring until the emulsifier is uniformly distributed in the water, sequentially adding methyl methacrylate, acrylic ester, acrylic acid, hydroxyethyl methacrylate, methacrylamide and an initiator, and stirring for 10-20 minutes to obtain a uniformly mixed solution for later use;
s3: preparing an outer-layer pre-emulsion: adding water and an emulsifier into a container with metering stirring, then stirring until the emulsifier is uniformly distributed in the water, adding acrylate, methacrylamide and a silane coupling agent, and stirring for 10-20 minutes to obtain a uniformly mixed solution for later use;
s4: after the temperature of the kettle bottom solution is raised to 83-88 ℃, adding 5% of kernel pre-emulsion and an initiator, preserving the heat for 20-30 minutes, uniformly and quickly feeding the kernel pre-emulsion into the kettle bottom by using a constant flow pump after the heat preservation is finished, keeping the dripping time at 120 minutes, and controlling the reaction temperature in the kettle at 85-88 ℃; after the dripping is finished, keeping the temperature for 0.5 hour, after the heat preservation is finished, dripping the outer-layer pre-emulsion for 60 minutes, keeping the temperature constant, and keeping the temperature for 0.5 hour after the dripping is finished;
s5: and (3) post-treatment of the emulsion: after the heat preservation is finished, cooling to 60-65 ℃, then simultaneously dripping an oxidant and a reducing agent, and preserving the heat for 10-15 minutes after finishing dripping;
s6: and after the heat preservation is finished, cooling to 50 ℃, then adjusting the pH value to 7-8 by using ammonia water, stirring for 30 minutes, filtering and discharging to obtain the novel real stone paint emulsion.
3. The weather-resistant real stone paint emulsion as claimed in claim 1, wherein: the alkenoic acid ester is at least one selected from isobutyl methacrylate or isobutyl acrylate.
4. The weather-resistant real stone paint emulsion as claimed in claim 1, wherein: the emulsifier is selected from at least one of ammonium vinylpolyoxyethylene alkyl thionate or disodium sulfosuccinate.
5. The weather-resistant real stone paint emulsion as claimed in claim 1, wherein: the alkyl carboxylic acid crosslinking monomer is at least one selected from acrylic acid, methacrylic acid and itaconic acid.
6. The weather-resistant real stone paint emulsion as claimed in claim 1, wherein: the silane coupling agent is at least one selected from vinyl trimethoxy silane and vinyl triethoxy silane.
7. The weather-resistant real stone paint emulsion as claimed in claim 1, wherein: the initiator is selected from at least one of ammonium persulfate, sodium persulfate or potassium persulfate.
8. The weather-resistant real stone paint emulsion as claimed in claim 1, wherein: the oxidant is selected from a tert-butyl hydroperoxide solution with the mass fraction of 5%, and the reducing agent is selected from a sodium formaldehyde sulfoxylate solution with the mass fraction of 5%.
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| CN202010078824.6A CN111138599A (en) | 2020-02-03 | 2020-02-03 | Preparation method of weather-resistant real stone paint emulsion |
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| CN202010078824.6A CN111138599A (en) | 2020-02-03 | 2020-02-03 | Preparation method of weather-resistant real stone paint emulsion |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112646445A (en) * | 2020-12-22 | 2021-04-13 | 衡水新光新材料科技有限公司 | Preparation method of real stone paint emulsion |
| CN113683935A (en) * | 2021-09-01 | 2021-11-23 | 佛山罗斯夫科技有限公司 | Pure acrylic flexible real stone paint emulsion and preparation method thereof |
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| CN112646445A (en) * | 2020-12-22 | 2021-04-13 | 衡水新光新材料科技有限公司 | Preparation method of real stone paint emulsion |
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