CN114230734A - Emulsion for texture paint, preparation method and application thereof - Google Patents
Emulsion for texture paint, preparation method and application thereof Download PDFInfo
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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
- C08F285/00—Macromolecular compounds obtained by polymerising monomers on to preformed graft polymers
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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
- C08F2/00—Processes of polymerisation
- C08F2/12—Polymerisation in non-solvents
- C08F2/16—Aqueous medium
- C08F2/22—Emulsion polymerisation
- C08F2/24—Emulsion polymerisation with the aid of emulsifying agents
- C08F2/26—Emulsion polymerisation with the aid of emulsifying agents anionic
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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
- C08F257/00—Macromolecular compounds obtained by polymerising monomers on to polymers of aromatic monomers as defined in group C08F12/00
- C08F257/02—Macromolecular compounds obtained by polymerising monomers on to polymers of aromatic monomers as defined in group C08F12/00 on to polymers of styrene or alkyl-substituted styrenes
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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
- C08F4/00—Polymerisation catalysts
- C08F4/28—Oxygen or compounds releasing free oxygen
- C08F4/30—Inorganic compounds
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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
- C08F4/00—Polymerisation catalysts
- C08F4/40—Redox systems
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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
Abstract
The invention discloses an emulsion for a texture coating, a preparation method and application thereof, wherein the emulsion comprises a three-layer core-shell structure which comprises a core layer, a transition layer and a shell layer from inside to outside in sequence, wherein the core layer and the transition layer comprise an acrylate monomer, styrene, an emulsifier, tert-butyl hydroperoxide and a reducing agent; the shell layer contains acrylate monomer, emulsifier and persulfate. The texture coating material has the advantages that the characteristics of a texture coating material formula are comprehensively considered, the three-layer core-shell structure emulsion, the gradual change distribution of functional monomers and the combination of different emulsion polymerization methods are respectively adopted, the emulsion is ensured to have enough toughness and proper branching degree distribution, an effective continuous compact film is formed in the film forming process of the emulsion, the water resistance of the emulsion can be fully improved, and the water absorption capacity of the emulsion can be reduced. On the other hand, the functional monomers are distributed in a gradual change manner, so that the functional monomers can have better adhesive force with a base material, and simultaneously, the surface tension in the film forming process can be adjusted, so that the functional monomers and the pigment and filler can be better dispersed, and the dry-wet color difference before and after texture coating construction and the color difference before and after water resistance can be reduced.
Description
Technical Field
The invention relates to the technical field of coatings, relates to an emulsion for a coating and a preparation method thereof, and particularly relates to an emulsion for a texture coating, a preparation method and application thereof.
Background
The texture coating is a coating material coated on a wall, has a realistic texture, is a very popular architectural wall decoration and protection coating at home and abroad in recent years, and can be rapidly developed and comprehensively popularized and applied in China at present. The texture coating is free of radiation and light in self weight, shows a unique space visual angle by means of infinite three-dimensional texture and multi-choice individual matching, is rich and vivid, is novel, economical and environment-friendly, and is widely applied to walls of buildings such as houses, villas, theme companies and office buildings. Therefore, the texture coating is very popular with consumers, and is now the trend of the coating industry.
The texture coating is mainly prepared by taking emulsion as a binder and quartz sand as main aggregate and adding a plurality of auxiliary agents. The emulsion is the key point for determining the performance of the latex paint for the outer wall, compared with the common outer wall paint, the texture paint has higher requirement on the emulsion, because the proportion of sand added in the whole paint formula is higher, the coating cannot be very compact, in addition, because the emulsion particles are incompletely fused into a film, moisture can permeate through capillaries among emulsion particle gaps, particularly under the condition of higher concentration of the emulsifier, the moisture can diffuse into the emulsion particles, and because micropores of the emulsion film expand along with the water absorption expansion of water-soluble substances, the water can permeate through capillary channels more easily, so the water absorption capacity becomes larger. Therefore, when an emulsion is selected as the texture paint, the water resistance tends to be higher than that of a general type of paint. Therefore, the texture coating has better performances such as water resistance, adhesion, wear resistance and the like besides the performances such as stain resistance, rain mark resistance and the like required by the common exterior wall coating.
Conventional core-shell structures, often two-layer structures, are generally used for conventional coating emulsions. In the practical application process, the core-shell structure of the two layers is easy to cause phase separation in the film forming process. The core part and the shell part cannot be well fused to form a better continuous phase along with the continuous volatilization of water in the film forming process due to the reasons of different glass transition temperatures, different monomer ratios, different acid distribution, different surface tensions and the like, so that the real benefits brought by the core-shell structure cannot be fully exerted, and the negative effects on water resistance and adhesive force are realized in the practical application of the texture coating.
Disclosure of Invention
In order to overcome the defects of low water resistance and low adhesive force with a base material after the film formation of the emulsion for the texture coating in the prior art, the invention researches according to the characteristics of a texture coating formula and provides the emulsion for the texture coating and a preparation method thereof.
In order to achieve the purpose, the technical scheme of the invention is as follows:
the emulsion comprises a three-layer core-shell structure, namely a core layer, a transition layer and a shell layer from inside to outside, wherein the core layer and the transition layer contain an acrylate monomer, styrene, an emulsifier, tert-butyl hydroperoxide and a reducing agent; the shell layer contains acrylate monomer, emulsifier and persulfate.
In certain embodiments, the core layer further comprises a silane coupling agent 174.
In certain embodiments, the acrylate monomer in the core layer and the transition layer is one or more of butyl acrylate, isooctyl acrylate, glycidyl methacrylate, acrylic acid, acrylonitrile, acrylamide.
In certain embodiments, the acrylate monomer in the shell layer is one or more of methyl methacrylate, butyl acrylate, isooctyl acrylate, methacrylic acid, acrylamide.
In certain embodiments, the reducing agent is one or more of the foregoing paullinia cupertiana SFS, sodium bisulfite, sodium ascorbate, brungelmann Bruggolite FF 6M.
In certain embodiments, the persulfate is one or both of potassium persulfate and sodium persulfate.
In certain embodiments, the emulsifier is one or more of a sulfonate anionic emulsifier, a phosphate anionic emulsifier, a polymerizable emulsifier.
In certain embodiments, the sulfonate anionic emulsifier is sodium dodecylbenzenesulfonate.
In certain embodiments, the phosphate anionic emulsifier is one or both of RS610, RS 710.
In certain embodiments, the polymerizable emulsifier is one or more of the emulsifiers SR10, ER10, AR10 with double bonds copolymerizable with the monomer.
In certain embodiments, the composition comprises, in weight percent:
12 to 22 percent of water in the nuclear layer, 0.2 to 1.2 percent of emulsifier, 0.05 to 0.5 percent of tert-butyl hydroperoxide, 0.1 to 0.8 percent of reducing agent, 3 to 11 percent of styrene, 0.5 to 10 percent of butyl acrylate, 0.5 to 10 percent of isooctyl acrylate, 0.1 to 2 percent of acrylic acid, 0 to 2 percent of glycidyl methacrylate GMA, 0.1 to 2 percent of acrylonitrile, 0 to 0.5 percent of acrylamide and 0 to 0.5 percent of silane coupling agent 174;
6-11% of water in the transition layer, 0.1-0.6% of emulsifier, 0.03-0.3% of tert-butyl hydroperoxide, 0.05-0.4% of reducing agent, 1.5-10% of styrene, 0.1-2% of butyl acrylate, 0.2-5% of isooctyl acrylate, 0.05-0.5% of acrylic acid, 0-1% of glycidyl methacrylate, 0.05-1% of acrylonitrile and 0-0.25% of acrylamide;
the shell layer contains 12 to 22 percent of water, 0.2 to 1.2 percent of emulsifier, 0.1 to 0.5 percent of persulfate, 7 to 15 percent of methyl methacrylate, 0.5 to 5 percent of butyl acrylate, 0.5 to 5 percent of isooctyl acrylate, 0.1 to 2 percent of methacrylic acid and 0 to 0.5 percent of acrylamide.
In a second aspect, the invention discloses a preparation method of an emulsion for a texture coating, which comprises the following steps:
(1) putting an emulsifier and water into a pre-emulsifier, stirring uniformly, and adding a monomer while stirring to respectively obtain a core layer monomer pre-emulsion, a transition layer monomer pre-emulsion and a shell layer monomer pre-emulsion;
(2) adding water into tert-butyl hydroperoxide to prepare an initiator solution, adding water into a reducing agent to prepare a reducing agent solution, and adding water into persulfate of the shell layer to prepare a persulfate solution.
(3) Putting water into a reaction kettle, heating to raise the temperature, simultaneously dropwise adding the monomer pre-emulsion of the nuclear layer, the tert-butyl hydroperoxide solution and the reducing agent solution, and after dropwise adding, preserving the heat;
(4) dripping the monomer pre-emulsion, the tert-butyl hydroperoxide solution and the reducing agent solution of the transition layer into the polymer emulsion in the step (3) at the same time, and preserving heat after dripping;
(5) heating the reaction, starting to dropwise add the monomer pre-emulsion and persulfate solution of the shell layer, and preserving heat after dropwise adding; and cooling the reaction temperature to room temperature, adjusting the pH value of the emulsion, filtering and discharging to obtain the texture coating emulsion.
In certain embodiments, the amount of water in step (3) is 20-40% of the total weight, the temperature is raised to 60-70 ℃, the reaction dropwise addition time is 1h, and the heat preservation time is 15 min.
In certain embodiments, the reaction is added dropwise for 30min and incubated for 15min in step (4).
In certain embodiments, the reaction in step (5) is heated to 80-85 ℃, the reaction dropping time is 1h, and the holding time is 30 min.
In certain embodiments, the emulsion pH is adjusted to 7-8 and the discharge is filtered.
In a third aspect, the invention discloses an application of the emulsion for texture paint or the emulsion for texture paint prepared by the preparation method, and the emulsion is used in a formula of architectural texture paint.
The invention has the following beneficial effects:
(1) the emulsion for texture coating has a three-layer core-shell structure, ensures the emulsion to have enough toughness and proper branching degree distribution, so that the emulsion forms an effective continuous compact film in the film forming process, and the water resistance of the emulsion can be fully improved.
(2) The emulsion for texture paint forms gradual change distribution of functional monomers, so that the emulsion can have better adhesive force with a base material, and simultaneously can adjust the surface tension in the film forming process, so that the emulsion and pigments and fillers can be better dispersed, and the dry-wet color difference before and after texture paint construction and the color difference before and after water resistance can be reduced. Functional monomers with polar groups, such as glycidyl methacrylate, silane coupling agent 174 and acrylonitrile, are introduced into the core layer to improve the adhesion with the substrate; the introduction of the functional monomers in the transition layer is reduced, so that the polymerization amount of the functional monomers on the outer layer is gradually reduced on one hand, and the surface tension of the emulsion is also adjusted on the other hand; functional monomers are not added into the shell layer, and the hydrophilicity of the emulsion is adjusted by adjusting the amount of acid, such as the distribution of methacrylic acid, so that the film formation of the emulsion is ensured, the distribution of the outer layer of the hydrophilic monomers is reduced, and the water resistance of the whole emulsion is improved.
(3) The emulsion with the three-layer core-shell structure adopts different polymerization methods, low-temperature redox polymerization is used in the polymerization process of the core layer and the transition layer, and high-temperature heat is used for initiating polymerization when the temperature of the shell layer is raised. In the conventional emulsion polymerization process, one initiation mode is often used, and the advantages of the two different initiation modes can be fully utilized by combining the two different initiation methods. The first two layers are subjected to low-temperature redox polymerization, so that a structure with larger molecular weight can be formed, and the emulsion has better toughness; the branching degree of the emulsion is improved by the outer layer thermal initiation, a structure with small molecular weight is formed, the film forming property and the fluidity of the emulsion are further improved, two structures with different molecular weight distributions can exert a synergistic effect, and the overall performance of the emulsion is improved.
(4) The invention fully considers the characteristics of the texture coating formula, and the prepared emulsion can well balance the overall performance of the texture coating by combining the three-layer core-shell structure emulsion, the gradual change distribution of functional monomers and different emulsion polymerization methods.
Detailed Description
The present invention will be described in further detail with reference to examples.
Example 1
The emulsion for the texture paint comprises the following components in parts by weight:
a nuclear layer: 120 parts of water, 2 parts of sodium dodecyl benzene sulfonate, 0.5 part of tert-butyl hydroperoxide, 1 part of Sodium Formaldehyde Sulfoxylate (SFS), 30 parts of styrene, 10 parts of butyl acrylate, 10 parts of isooctyl acrylate, 2 parts of glycidyl methacrylate, 1 part of acrylic acid, 1 part of acrylonitrile and 1741 parts of silane coupling agent;
transition layer: 60 parts of water, RS 6101 parts, 0.3 part of tert-butyl hydroperoxide, 0.5 part of sodium formaldehyde sulfoxylate SFS, 15 parts of styrene, 3 parts of butyl acrylate, 5 parts of isooctyl acrylate, 0.5 part of acrylic acid and 0.5 part of acrylonitrile;
shell layer: 160 parts of water, 105 parts of SR, 2.5 parts of sodium persulfate, 100 parts of methyl methacrylate, 50 parts of butyl acrylate, 50 parts of isooctyl acrylate, 10 parts of methacrylic acid and 2 parts of acrylamide.
The preparation method of the emulsion for texture paint of the embodiment comprises the following steps:
(1) weighing 90-95% of water in the first layer and all the emulsifier according to the weight ratio of the formula, placing the mixture in a beaker, uniformly stirring, sequentially adding the monomers of the core layer while stirring to prepare a core layer monomer pre-emulsion, wherein the preparation methods of the transition layer monomer pre-emulsion and the shell layer monomer pre-emulsion are the same as those of the core layer monomer pre-emulsion;
(2) adding tert-butyl hydroperoxide and a reducing agent into the residual water of the nuclear layer and the transition layer respectively, and stirring uniformly; and adding the persulfate of the shell layer into the residual water amount of the shell layer, and uniformly stirring.
(3) Adding water accounting for 20-40% of the total weight into a reaction kettle, heating to 60-70 ℃, simultaneously dropwise adding the monomer pre-emulsion of the nuclear layer, the tert-butyl hydroperoxide solution and the reducing agent solution, and keeping the temperature for 15 minutes after dropwise adding is finished within 1 hour;
(4) dripping the monomer pre-emulsion, the tert-butyl hydroperoxide solution and the reducing agent solution of the transition layer into the polymer emulsion in the step (3), and preserving heat for 15 minutes after dripping within 30 minutes;
(5) heating the reaction to 80-85 ℃, starting to dropwise add the monomer pre-emulsion and persulfate solution of the shell layer, and keeping the temperature for 30 minutes after dropwise addition is finished within 1 hour; and cooling the reaction temperature to room temperature, adjusting the pH value of the emulsion to 7-8, filtering and discharging to obtain the emulsion for the texture coating.
Example 2
The emulsion for the texture paint comprises the following components in parts by weight:
a nuclear layer: 120 parts of water, 1 part of RS 7105, 1 part of tert-butyl hydroperoxide, 2 parts of sodium bisulfite, 30 parts of styrene, 15 parts of butyl acrylate, 15 parts of isooctyl acrylate, 5 parts of acrylic acid, 5 parts of acrylonitrile and 1.5 parts of acrylamide;
transition layer: 110 parts of water, RS 7106 parts of tert-butyl hydroperoxide, 3 parts of Bruggolite FF6M 4 parts of Bruggolite, 70 parts of styrene, 10 parts of butyl acrylate, 50 parts of isooctyl acrylate, 5 parts of acrylic acid, 5 parts of glycidyl methacrylate, 10 parts of acrylonitrile and 2.5 parts of acrylamide;
shell layer: 120 parts of water, 102 parts of ER, 1 part of potassium persulfate, 70 parts of methyl methacrylate, 25 parts of butyl acrylate, 25 parts of isooctyl acrylate and 1 part of methacrylic acid.
The preparation method of the emulsion for texture paint of this example is the same as that of example 1.
Example 3
The emulsion for the texture paint comprises the following components in parts by weight:
a nuclear layer: 140 parts of water, RS 7106 parts, 2 parts of tert-butyl hydroperoxide, 4 parts of sodium ascorbate, 60 parts of styrene, 30 parts of butyl acrylate, 30 parts of isooctyl acrylate, 5 parts of acrylic acid, 6 parts of glycidyl methacrylate, 6 parts of acrylonitrile and 2 parts of acrylamide.
Transition layer: 80 parts of water, RS 7103 parts, 1 part of tert-butyl hydroperoxide, 2 parts of sodium ascorbate, 40 parts of styrene, 8 parts of butyl acrylate, 10 parts of isooctyl acrylate, 2.5 parts of acrylic acid, 5 parts of glycidyl methacrylate, 5 parts of acrylonitrile and 1.5 parts of acrylamide;
shell layer: 140 parts of water, 2.5 parts of RS 7105 parts of potassium persulfate, 80 parts of methyl methacrylate, 35 parts of butyl acrylate, 45 parts of isooctyl acrylate, 10 parts of methacrylic acid and 2.5 parts of acrylamide.
The preparation method of the emulsion for texture paint of this example is the same as that of example 1.
Comparative example 1
The emulsion comprises the following components in parts by weight:
a nuclear layer: 180 parts of water, 3 parts of sodium dodecyl benzene sulfonate, 0.8 part of tert-butyl hydroperoxide, 1.5 parts of Sodium Formaldehyde Sulfoxylate (SFS), 45 parts of styrene, 13 parts of butyl acrylate, 5 parts of isooctyl acrylate, 2 parts of glycidyl methacrylate, 1.5 parts of acrylic acid, 1.5 parts of acrylonitrile and 1741 parts of silane coupling agent;
shell layer: 160 parts of water, 105 parts of SR, 2.5 parts of sodium persulfate, 100 parts of methyl methacrylate, 50 parts of butyl acrylate, 50 parts of isooctyl acrylate, 10 parts of methacrylic acid and 2 parts of acrylamide.
The preparation method of this example includes the following steps:
(1) weighing 90-95% of water in the core layer and all the emulsifier according to the weight ratio of the formula, placing the mixture in a beaker, uniformly stirring, and sequentially adding the monomers while stirring to respectively prepare the core layer monomer pre-emulsion and the shell layer monomer pre-emulsion.
(2) And respectively adding tert-butyl hydroperoxide and a reducing agent into the rest amount of water, and uniformly stirring.
(3) Adding water accounting for 20-40% of the total weight into a reaction kettle, heating to 60-70 ℃, simultaneously dropwise adding the nuclear layer monomer pre-emulsion, the tert-butyl hydroperoxide solution and the reducing agent solution, and keeping the temperature for 15 minutes after dropwise adding is completed within 1 hour;
(4) heating the reaction to 80-85 ℃, starting to dropwise add the monomer pre-emulsion and persulfate solution of the shell layer, and keeping the temperature for 30 minutes after dropwise adding is finished within 1 hour; cooling the reaction temperature to room temperature, adjusting the pH value of the emulsion to 7-8, filtering and discharging.
Comparative example 2
The emulsion comprises the following components in parts by weight:
a nuclear layer: 120 parts of water, 2 parts of sodium dodecyl benzene sulfonate, 0.5 part of tert-butyl hydroperoxide, 1 part of Sodium Formaldehyde Sulfoxylate (SFS), 30 parts of styrene, 10 parts of butyl acrylate, 10 parts of isooctyl acrylate, 2 parts of glycidyl methacrylate, 1 part of acrylic acid, 1 part of acrylonitrile and 1741 parts of silane coupling agent;
transition layer: 60 parts of water, RS 6101 parts, 0.3 part of tert-butyl hydroperoxide, 0.5 part of sodium formaldehyde sulfoxylate SFS, 15 parts of styrene, 3 parts of butyl acrylate, 5 parts of isooctyl acrylate, 2 parts of glycidyl methacrylate, 1 part of acrylic acid, 1 part of acrylonitrile and 1741 parts of silane coupling agent;
shell layer: 160 parts of water, 105 parts of SR, 2.5 parts of sodium persulfate, 100 parts of methyl methacrylate, 50 parts of butyl acrylate, 50 parts of isooctyl acrylate, 2 parts of glycidyl methacrylate, 1 part of acrylic acid, 1 part of acrylonitrile and 1741 parts of silane coupling agent.
The preparation method of this example includes the following steps:
(1) weighing 90-95% of water in the first layer and all the emulsifier according to the weight ratio of the formula, placing the mixture in a beaker, uniformly stirring, sequentially adding the monomers of the core layer while stirring to prepare a core layer monomer pre-emulsion, wherein the preparation methods of the transition layer monomer pre-emulsion and the shell layer monomer pre-emulsion are the same as those of the core layer monomer pre-emulsion;
(2) adding tert-butyl hydroperoxide and a reducing agent into the residual water of the nuclear layer and the transition layer respectively, and stirring uniformly; and adding the persulfate of the shell layer into the residual water amount of the shell layer, and uniformly stirring.
(3) Adding water accounting for 20-40% of the total weight into a reaction kettle, heating to 60-70 ℃, simultaneously dropwise adding the nuclear layer monomer pre-emulsion, the tert-butyl hydroperoxide solution and the reducing agent solution, and keeping the temperature for 15 minutes after dropwise adding is completed within 1 hour;
(4) dripping the monomer pre-emulsion, the tert-butyl hydroperoxide solution and the reducing agent solution of the transition layer into the polymer emulsion in the step (3), and preserving heat for 15 minutes after dripping within 30 minutes;
(5) heating the reaction to 80-85 ℃, starting to dropwise add the monomer pre-emulsion and persulfate solution of the shell layer, and keeping the temperature for 30 minutes after dropwise addition is finished within 1 hour; cooling the reaction temperature to room temperature, adjusting the pH value of the emulsion to 7-8, filtering and discharging.
Comparative example 3
The emulsion comprises the following components in parts by weight:
a nuclear layer: 120 parts of water, 2 parts of sodium dodecyl benzene sulfonate, 0.5 part of tert-butyl hydroperoxide, 1 part of Sodium Formaldehyde Sulfoxylate (SFS), 30 parts of styrene, 10 parts of butyl acrylate, 10 parts of isooctyl acrylate, 2 parts of glycidyl methacrylate, 1 part of acrylic acid, 1 part of acrylonitrile and 1741 parts of silane coupling agent;
transition layer: 60 parts of water, RS 6101 parts, 0.3 part of tert-butyl hydroperoxide, 0.5 part of sodium formaldehyde sulfoxylate SFS, 15 parts of styrene, 3 parts of butyl acrylate, 5 parts of isooctyl acrylate, 0.5 part of acrylic acid and 0.5 part of acrylonitrile;
shell layer: 160 parts of water, 105 parts of SR, 0.5 part of tert-butyl hydroperoxide, 1 part of sodium formaldehyde sulfoxylate SFS, 100 parts of methyl methacrylate, 50 parts of butyl acrylate, 50 parts of isooctyl acrylate, 10 parts of methacrylic acid and 2 parts of acrylamide.
The preparation method of this example includes the following steps:
(1) weighing 90-95% of water in the first layer and all the emulsifier according to the weight ratio of the formula, placing the mixture in a beaker, uniformly stirring, sequentially adding the monomers of the core layer while stirring to prepare a core layer monomer pre-emulsion, wherein the preparation methods of the transition layer monomer pre-emulsion and the shell layer monomer pre-emulsion are the same as those of the core layer monomer pre-emulsion;
(2) and (3) adding tert-butyl hydroperoxide and a reducing agent into the residual water of the core layer, the transition layer and the shell layer respectively, and stirring uniformly.
(3) Adding water accounting for 20-40% of the total weight into a reaction kettle, heating to 60-70 ℃, simultaneously dropwise adding the nuclear layer monomer pre-emulsion, the tert-butyl hydroperoxide solution and the reducing agent solution, and keeping the temperature for 15 minutes after dropwise adding is completed within 1 hour;
(4) dripping the monomer pre-emulsion, the tert-butyl hydroperoxide solution and the reducing agent solution of the transition layer into the polymer emulsion in the step (3), and preserving heat for 15 minutes after dripping within 30 minutes;
(5) dropping the monomer pre-emulsion, the tert-butyl hydroperoxide solution and the reducing agent solution of the shell layer, and keeping the temperature for 30 minutes after dropping within 1 hour; cooling the reaction temperature to room temperature, adjusting the pH value of the emulsion to 7-8, filtering and discharging.
Performance testing
Texture paint was prepared according to the following formulation in examples 1 to 3 and comparative examples 1 to 3, respectively.
The texture coating comprises the following specific implementation formula in parts by weight: 120 parts of emulsion, 10 ten thousand HPMC2 parts, 0.5 part of 250HBR, 5 parts of bentonite, AMP-951 parts, SN-50404 parts, TO-81 parts, NXZ 2 parts, 10 parts of glycol, R-81830 parts, CC-70070 parts, C-128.4 parts, TT-9353 parts, 600 parts of 46-60-mesh sand and 140 parts of water.
The inventive examples and comparative examples were compared according to the relevant standards, and the measured performance indexes are shown in table 1.
TABLE 1 Performance test indices for textured coatings prepared from different emulsions
Remarking:
water absorption test method: according to the water permeability test method in the national standard JG/T210-2018.
The adhesion test method comprises the following steps: adding 30% of water into the prepared paint, uniformly stirring, uniformly coating on a prepared putty plate, pasting gummed paper after 24 hours, pulling off with force, and if the paint film does not fall off, judging that the adhesive force is excellent, and evaluating the adhesive force as grade 5; if the paint film completely falls off, the adhesive force is poor, and the evaluation is 0 grade; the rest of the tests were evaluated between the 0 to 5 grades according to the falling-off of the paint film.
The color spreading test method comprises the following steps: adding 1% of color paste into a certain amount of paint, fully stirring uniformly, then carrying out blade coating on a glass plate by using a wet film coater to form a film with the thickness of 400 mu m, starting to grind the periphery of the paint film until the paint film is dried, firstly measuring the part without grinding by using a color difference meter to prepare a standard sample, then measuring the position of grinding, and obtaining a result by comparing the positions by using the color difference meter.
Water resistance is the resistance of the coating film to the action of water, namely the performance of water impermeability without water absorption, and the water resistance of the emulsion directly influences the water resistance of the coating. As can be seen from the test data in Table 1, in the water absorption test, the water absorption of the texture coating prepared from the emulsion of the invention is relatively low, which indicates that the emulsion of the invention forms a continuous effective compact film in the film forming process, and sand grains are packed more tightly, thereby improving the water resistance of the film and reducing the water absorption of the film.
The emulsion of the invention forms the gradual distribution of the functional monomer, so that the emulsion can have better adhesive force with the base material. As can be seen from the test data in table 1, the coating films prepared therefrom have good adhesion.
The common color difference in the practical application of the paint is mostly caused by poor water resistance of the emulsion, and the color difference before and after the water of the coating film can be seen to be relatively low, so that the color difference before and after the water of the texture paint coating prepared by the emulsion is relatively low, and the emulsion for the texture paint prepared by the invention has better water resistance.
The emulsion in comparative example 1 is a traditional two-layer core-shell structure, the monomers of each layer of the emulsion in comparative example 2 are the same, and the emulsion in comparative example 3 adopts only one polymerization mode. The texture coating material comprehensively considers the characteristics of a texture coating material formula, and the emulsion with a three-layer core-shell structure, the gradual change distribution of functional monomers and the combination of different emulsion polymerization methods have proper branching degree distribution while ensuring enough toughness of the emulsion, so that the emulsion effectively forms a continuous and compact film in the film forming process, the water resistance of the emulsion can be fully improved, and the water absorption capacity can be reduced. On the other hand, the functional monomers are distributed in a gradual change manner, so that the functional monomers have better adhesive force with a base material, and simultaneously, the surface tension in the film forming process can be adjusted, so that the functional monomers and the pigments and fillers can be better dispersed, and the dry and wet color difference degree before and after texture coating construction and the color difference degree before and after water resistance can be reduced.
The foregoing is directed to embodiments of the present invention, and it is understood that various changes and modifications may be made therein by those skilled in the art without departing from the spirit and scope of the invention.
Claims (10)
1. The emulsion for the texture coating is characterized by comprising a three-layer core-shell structure, namely a core layer, a transition layer and a shell layer from inside to outside, wherein the core layer and the transition layer comprise an acrylate monomer, styrene, an emulsifier, tert-butyl hydroperoxide and a reducing agent; the shell layer contains acrylate monomer, emulsifier and persulfate.
2. A textured coating emulsion as claimed in claim 1 wherein said core layer further comprises a silane coupling agent 174; the acrylate monomer in the core layer and the transition layer is one or more of butyl acrylate, isooctyl acrylate, glycidyl methacrylate, acrylic acid, acrylonitrile and acrylamide; the acrylate monomer in the shell layer is one or more of methyl methacrylate, butyl acrylate, isooctyl acrylate, methacrylic acid and acrylamide.
3. A textured coating emulsion as claimed in claim 1 wherein said reducing agent is one or more of the group consisting of Sodium Formaldehyde Sulfoxylate (SFS), sodium bisulfite, sodium ascorbate, Bruggolite FF 6M.
4. A textured coating emulsion as claimed in claim 1 wherein said persulfate is one or both of potassium persulfate and sodium persulfate.
5. A textured coating emulsion as claimed in claim 1 wherein said emulsifier is one or more of a sulfonate anionic emulsifier, a phosphate anionic emulsifier, a polymerizable emulsifier.
6. A textured coating emulsion as claimed in claim 5 wherein said sulfonate anionic emulsifier is sodium dodecylbenzene sulfonate; the phosphate anionic emulsifier is one or two of RS610 and RS 710; the polymerizable emulsifier is one or more of emulsifiers SR10, ER10 and AR10 which have double bonds and can be copolymerized with monomers.
7. A textured coating emulsion as claimed in claim 2 wherein the weight percent:
the core layer contains 12 to 22 percent of water, 0.2 to 1.2 percent of emulsifier, 0.05 to 0.5 percent of tert-butyl hydroperoxide, 0.1 to 0.8 percent of reducing agent, 3 to 11 percent of styrene, 0.5 to 10 percent of butyl acrylate, 0.5 to 10 percent of isooctyl acrylate, 0.1 to 2 percent of acrylic acid, 0 to 2 percent of glycidyl methacrylate, 0.1 to 2 percent of acrylonitrile, 0 to 0.5 percent of acrylamide and 0 to 0.5 percent of silane coupling agent 174;
the transition layer contains 6 to 11 percent of water, 0.1 to 0.6 percent of emulsifier, 0.03 to 0.3 percent of tert-butyl hydroperoxide, 0.05 to 0.4 percent of reducing agent, 1.5 to 10 percent of styrene, 0.1 to 2 percent of butyl acrylate, 0.2 to 5 percent of isooctyl acrylate, 0.05 to 0.5 percent of acrylic acid, 0 to 1 percent of glycidyl methacrylate, 0.05 to 1 percent of acrylonitrile and 0 to 0.25 percent of acrylamide;
the shell layer contains 12-22% of water, 0.2-1.2% of emulsifier, 0.1-0.5% of persulfate, 7-15% of methyl methacrylate, 0.5-5% of butyl acrylate, 0.5-5% of isooctyl acrylate, 0.1-2% of methacrylic acid and 0-0.5% of acrylamide.
8. A method of preparing an emulsion for texture coating as claimed in claim 7, comprising the steps of:
(1) putting an emulsifier and water into a pre-emulsifier, stirring uniformly, and adding a monomer while stirring to respectively obtain a core layer monomer pre-emulsion, a transition layer monomer pre-emulsion and a shell layer monomer pre-emulsion;
(2) adding water into tert-butyl hydroperoxide to prepare an initiator solution, adding water into a reducing agent to prepare a reducing agent solution, and adding water into persulfate of the shell layer to prepare a persulfate solution.
(3) Putting water into a reaction kettle, heating to raise the temperature, simultaneously dropwise adding the monomer pre-emulsion of the nuclear layer, the tert-butyl hydroperoxide solution and the reducing agent solution, and after dropwise adding, preserving the heat;
(4) dripping the monomer pre-emulsion, the tert-butyl hydroperoxide solution and the reducing agent solution of the transition layer into the polymer emulsion in the step (3) at the same time, and preserving heat after dripping;
(5) heating the reaction, starting to dropwise add the monomer pre-emulsion and persulfate solution of the shell layer, and preserving heat after dropwise adding; and cooling the reaction temperature to room temperature, adjusting the pH value of the emulsion, filtering and discharging to obtain the texture coating emulsion.
9. A preparation method of emulsion for texture paint as claimed in claim 8, wherein in the step (3), the water amount accounts for 20-40% of the total weight, the temperature is raised to 60-70 ℃, the dropping time of the reaction is 1h, and the holding time is 15 min; the reaction dripping time in the step (4) is 30min, and the heat preservation time is 15 min; and (3) heating the reaction in the step (5) to 80-85 ℃, dropwise adding the reaction for 1h, and keeping the temperature for 30 min.
10. A texture coating emulsion as claimed in any one of claims 1 to 7 wherein the emulsion is used in an architectural texture coating formulation.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115216256A (en) * | 2022-08-15 | 2022-10-21 | 衡水新光新材料科技有限公司 | High-performance ceramic tile binder |
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