CN113896827A - Acrylate microemulsion and preparation method thereof - Google Patents
Acrylate microemulsion and preparation method thereof Download PDFInfo
- Publication number
- CN113896827A CN113896827A CN202111020810.XA CN202111020810A CN113896827A CN 113896827 A CN113896827 A CN 113896827A CN 202111020810 A CN202111020810 A CN 202111020810A CN 113896827 A CN113896827 A CN 113896827A
- Authority
- CN
- China
- Prior art keywords
- parts
- reaction kettle
- emulsion
- initiator
- deionized water
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- 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
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/14—Methyl esters, e.g. methyl (meth)acrylate
-
- 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
-
- 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
- C08F2/30—Emulsion polymerisation with the aid of emulsifying agents non-ionic
-
- 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
- C08F2/38—Polymerisation using regulators, e.g. chain terminating agents, e.g. telomerisation
-
- 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
- C09D143/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and containing boron, silicon, phosphorus, selenium, tellurium, or a metal; Coating compositions based on derivatives of such polymers
- C09D143/04—Homopolymers or copolymers of monomers containing silicon
-
- 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
- C09D5/29—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes for multicolour effects
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Paints Or Removers (AREA)
Abstract
The invention discloses an acrylate microemulsion and a preparation method thereof, which are applied to multicolor coatings and comprise the following components in parts by weight: 100 parts of deionized water, 2-8 parts of composite emulsifier, 20-50 parts of methyl methacrylate, 20-60 parts of isooctyl acrylate, 20-50 parts of butyl methacrylate, 2-8 parts of acid monomer, 1-3 parts of amine monomer, 1-3 parts of crosslinking monomer, 0.1-0.5 part of initiator and 1-2 parts of pH regulator. The prepared acrylate microemulsion has better particle toughness and high shear stability.
Description
Technical Field
The invention relates to the technical field of architectural multicolor coatings, in particular to an acrylate microemulsion and a preparation method thereof.
Background
The colorful coating is used as an imitation granite coating, has light weight and convenient construction, overcomes the defects of heavy weight of granite, difficult construction and the like, and has the characteristics of water washing resistance, dirt resistance, strong wear resistance, strong acid and alkali resistance and the like. Therefore, the paint is widely applied to the surface of cement, stone surface, brick, wood, metal and the like as decoration.
Because the multicolor paint is a non-monochromatic product with various mixed particles, the manufacturing period is long, the method is precise and complex, various problems often occur in the manufacturing process, the stability of the product batch cannot be ensured, and the quality of the product is greatly influenced.
The existing multi-color paint particles on the market have insufficient toughness and poor high shear stability, and the color dots are easy to break after spraying and difficult to produce on a large scale, and the method is mainly related to the raw material acrylate emulsion in the multi-color paint.
Therefore, an acrylic ester emulsion for multicolor paint with good particle toughness and good high shear stability is urgently needed.
Disclosure of Invention
The present disclosure is directed to solving at least one of the technical problems of the related art or related art.
To this end, in a first aspect of the present disclosure, there is provided a method for preparing an acrylate microemulsion, comprising:
a. preparing an initiator solution: mixing 20-40% of the total amount of the initiator and 3% of the total amount of the deionized water at normal temperature and normal pressure to form an initiator solution A; mixing 7% of the total amount of the deionized water with the rest of the initiator to form an initiator solution B for later use;
b. preparing a pre-emulsion: mixing 30-40% of deionized water, 70-80% of composite emulsifier, methyl methacrylate, isooctyl acrylate, butyl methacrylate, acid monomer, amine monomer and crosslinking monomer in a high-pressure homogenizer, pre-emulsifying, and homogenizing for 40min to obtain pre-emulsion;
c. preparing a seed emulsion: adding the balance of deionized water and the balance of composite emulsifier into a reaction kettle at normal temperature and normal pressure, uniformly stirring, raising the temperature in the kettle to be more than or equal to 78 ℃, then adding 5-10% of the total amount of the pre-emulsion into the reaction kettle, simultaneously adding an initiator solution A, controlling the temperature to be 80-86 ℃ and keeping the temperature for 30min to prepare the seed emulsion;
d. c, dropwise adding the rest of pre-emulsion into the reaction kettle in the step c at a constant speed, and simultaneously dropwise adding an initiator solution B into the reaction kettle at a constant speed for 2-3 h;
e. after the dropwise adding in the step d is finished, controlling the temperature in the reaction kettle to be 80-86 ℃, and preserving the heat for 1-2 hours;
f. and e, cooling the reaction kettle in the step e to be less than or equal to 40 ℃, adding a pH regulator into the reaction kettle, regulating the pH to be 7-9, stirring for 30min, filtering and discharging to prepare the acrylate microemulsion applied to the multicolor paint.
Further, the composite emulsifier comprises an anionic emulsifier and a nonionic emulsifier, wherein the mass ratio of the anionic emulsifier to the nonionic emulsifier is 1: 1 to 3.
Further, the anionic emulsifier is one or the mixture of dodecyl diphenyl ether sodium disulfonate, sulfosuccinic acid ethoxy ether lauryl monoester disodium salt and allyl ether hydroxypropyl sodium sulfonate in any proportion.
Further, the nonionic emulsifier is one of or a mixture of isomeric tridecanol polyoxyethylene ether, alkyl polyoxyethylene ether and methallyl alcohol polyoxyethylene ether in any proportion.
Further, the acid monomer is one of acrylic acid and methacrylic acid or the above components are mixed in any proportion.
Further, the amine monomer is one of or the mixture of the components of diethylaniline, diethylhydroxylamine and methyldiethanolamine in any proportion.
The crosslinking monomer is one or the mixture of allyl methacrylate, ethylene glycol dimethacrylate, vinyl trimethoxy silane and gamma-methacryloxypropyl trimethoxy silane in any proportion.
Further, the initiator is one or the mixture of ammonium persulfate, potassium persulfate and sodium persulfate in any proportion.
Further, the pH regulator is one of ammonia water and 2-amino-2-methyl-1-propanol or the mixture of the components in any proportion.
In a second aspect of the present disclosure, an acrylate microemulsion prepared according to the above-described preparation method is provided.
According to the technical scheme, the beneficial effects of the invention are as follows:
1. the prepared acrylic ester microemulsion adopts a special microemulsion polymerization process. Compared with the traditional polymerization process, the prepared microemulsion has smaller particle size, more excellent permeability and wettability and can obviously improve the adhesion of the coating to a base material; the molecular density of the surfactant on the surface of the emulsion particles of the microemulsion is obviously higher than that of the common emulsion, so that the emulsion particles are difficult to damage under the action of high shear, and the toughness and the stability of the colorful coating particles under the action of high shear are improved.
2. In the prepared acrylate microemulsion, an amine monomer is used. The amine monomer can adjust the hydrophilic-lipophilic property and/or polar amine in the emulsifier to ensure that the dispersed phase reaches molecular level dispersion, and fine emulsion particles are obtained after the continuous phase material is added; the amine monomer is the key to the preparation of thermodynamically stable microemulsions.
3. In the acrylate microemulsion prepared by the present invention, a large amount of polyfunctional crosslinking monomers (allyl methacrylate, ethylene glycol dimethacrylate, vinyltrimethoxysilane, gamma-methacryloxypropyltrimethoxysilane, etc.) are used. The high-crosslinking-degree crosslinking network formed by the multifunctional crosslinking monomer ensures that the micro latex particles of the microemulsion can keep a stable structure under the action of high shear without being damaged, thereby improving the toughness of the multicolor paint particles and the stability under the action of high shear; the multifunctional monomer generally refers to a compound containing 2 or more than 2 photoactive groups, and has the advantages of high curing speed, low volatility, capability of endowing a cured film with a cross-linked structure and the like.
Detailed Description
The principles and features of this invention are described below in conjunction with embodiments, which are included to explain the invention and not to limit the scope of the invention.
In addition, the term "and/or" herein is only one kind of association relationship describing an associated object, and means that there may be three kinds of relationships, for example, a and/or B, which may mean: a exists alone, A and B exist simultaneously, and B exists alone. In addition, the character "/" herein generally indicates that the former and latter related objects are in an "or" relationship.
The term ambient temperature and pressure as used in this disclosure generally refers to the temperature at which the reaction occurs under typical test conditions, e.g., temperature: 24 ℃, 25 ℃ or 26 ℃; air pressure: 1 standard atmospheric pressure plus or minus 20 percent, 1 standard atmospheric pressure is 1.01 multiplied by 10^5N per square meter (100kPa is 0.1 MPa).
The acrylate microemulsion prepared by the present disclosure is generally applied to multicolor coatings.
In order to make the objects, technical solutions and advantages of the present invention more apparent, the following detailed description of the embodiments is given with reference to table 1, but the present invention is not limited to the scope of the embodiments.
TABLE 1 (component units in parts by mass)
Example 1
In some embodiments, the acrylate microemulsion comprises deionized water, a composite emulsifier, methyl methacrylate, isooctyl acrylate, butyl methacrylate, an acid monomer, an amine monomer, a crosslinking monomer, an initiator, and a pH regulator, and the above components may be: 100 parts of deionized water, 2 parts of sodium dodecyl diphenyl ether disulfonate, 3 parts of isomeric tridecanol polyoxyethylene ether, 32 parts of methyl methacrylate, 26 parts of isooctyl acrylate, 9.3 parts of butyl methacrylate, 1.2 parts of acrylic acid, 1 part of allyl methacrylate, 1 part of vinyl trimethoxy silane, 0.05 part of diethylaniline, 0.2 part of potassium persulfate and 0.8 part of ammonia water.
Specifically, the acrylate microemulsion can be prepared by the following method:
a. preparation of initiator solution: and (2) taking 20% of the total amount of the initiator and 3% of the total amount of the deionized water in the formula, mixing to form an initiator solution A, and then dissolving the rest of the initiator in 7% of the total amount of the deionized water to form an initiator solution B for later use at normal temperature and normal pressure.
b. Preparation of pre-emulsion: taking 40% of the total amount of the deionized water, 80% of the total amount of the composite emulsifier, methyl methacrylate, isooctyl acrylate, butyl methacrylate, acid monomers, amine monomers and crosslinking monomers, mixing in a high-pressure homogenizer for pre-emulsification, and continuously homogenizing for 40min to prepare uniform pre-emulsion.
c. Preparing a seed emulsion: adding the balance of deionized water and the balance of composite emulsifier into a reaction kettle at normal temperature and normal pressure, stirring uniformly, heating until the temperature in the kettle reaches about 80 ℃, then adding 7 percent of the total amount of the pre-emulsion into the reaction kettle, simultaneously adding the initiator solution A, controlling the temperature at about 80 ℃ and keeping the temperature for 30min to prepare the seed emulsion.
d. And d, dropwise adding the rest of pre-emulsion into the reaction kettle in the step c at a constant speed, and dropwise adding the initiator solution B into the reaction kettle at a constant speed for 3 hours.
e. And d, after the dropwise adding in the step d is finished, controlling the temperature in the reaction kettle to be about 80 ℃, and preserving the temperature for 1 h.
f. And e, cooling the reaction kettle in the step e to 40 ℃, adding a pH regulator into the reaction kettle, regulating the pH to 8, stirring for 30min, filtering and discharging to prepare the acrylic ester microemulsion applied to the multicolor paint.
Example 2
In some embodiments, the acrylate microemulsion comprises deionized water, a composite emulsifier, methyl methacrylate, isooctyl acrylate, butyl methacrylate, an acid monomer, an amine monomer, a crosslinking monomer, an initiator, and a pH regulator, and the above components may be: 100 parts of deionized water, 2 parts of sulfosuccinic acid ethoxy ether lauryl monoester disodium salt, 3 parts of alkyl polyoxyethylene ether, 32.5 parts of methyl methacrylate, 26 parts of isooctyl acrylate, 8.8 parts of butyl methacrylate, 1 part of acrylic acid, 1 part of allyl methacrylate, 1 part of vinyl trimethoxy silane, 0.05 part of diethylaniline, 0.2 part of potassium persulfate and 0.8 part of ammonia water.
Specifically, the acrylate microemulsion can be prepared by the following method:
a. preparation of initiator solution: and (2) taking 20% of the total amount of the initiator and 3% of the total amount of the deionized water in the formula, mixing to form an initiator solution A, and then dissolving the rest of the initiator in 7% of the total amount of the deionized water to form an initiator solution B for later use at normal temperature and normal pressure.
b. Preparation of pre-emulsion: taking 40% of the total amount of the deionized water, 80% of the total amount of the composite emulsifier, methyl methacrylate, isooctyl acrylate, butyl methacrylate, acid monomers, amine monomers and crosslinking monomers, mixing in a high-pressure homogenizer for pre-emulsification, and continuously homogenizing for 40min to prepare uniform pre-emulsion.
c. Preparing a seed emulsion: adding the balance of deionized water and the balance of composite emulsifier into a reaction kettle at normal temperature and normal pressure, stirring uniformly, heating until the temperature in the kettle reaches about 84 ℃, then adding 7 percent of the total amount of the pre-emulsion into the reaction kettle, simultaneously adding the initiator solution A, controlling the temperature at about 84 ℃ and keeping the temperature for 30min to prepare the seed emulsion.
d. And d, dropwise adding the rest of pre-emulsion into the reaction kettle in the step c at a constant speed, and dropwise adding the initiator solution B into the reaction kettle at a constant speed for 3 hours.
e. And d, after the dropwise adding in the step d is finished, controlling the temperature in the reaction kettle to be about 84 ℃, and preserving the temperature for 1 h.
f. And e, cooling the reaction kettle in the step e to 40 ℃, adding a pH regulator into the reaction kettle, regulating the pH to 8, stirring for 30min, filtering and discharging to prepare the acrylic ester microemulsion applied to the multicolor paint.
Example 3
In some embodiments, the acrylate microemulsion comprises deionized water, a composite emulsifier, methyl methacrylate, isooctyl acrylate, butyl methacrylate, an acid monomer, an amine monomer, a crosslinking monomer, an initiator and a pH regulator, wherein the components in parts by mass are respectively as follows: 100 parts of deionized water, 1 part of sodium dodecyl diphenyl ether disulfonate, 1 part of sodium allyl ether hydroxypropyl sulfonate, 3 parts of methallyl alcohol polyoxyethylene ether, 30 parts of methyl methacrylate, 28 parts of isooctyl acrylate, 9.3 parts of butyl methacrylate, 1.5 parts of methacrylic acid, 1 part of allyl methacrylate, 1.2 parts of gamma-methacryloxypropyl trimethoxy silane, 0.03 part of diethyl hydroxylamine, 0.2 part of ammonium persulfate and 0.8 part of ammonia water.
Specifically, the acrylate microemulsion can be prepared by the following method:
a. preparation of initiator solution: and (2) taking 20% of the total amount of the initiator and 3% of the total amount of the deionized water in the formula, mixing to form an initiator solution A, and then dissolving the rest of the initiator in 7% of the total amount of the deionized water to form an initiator solution B for later use at normal temperature and normal pressure.
b. Preparation of pre-emulsion: taking 40% of the total amount of the deionized water, 75% of the total amount of the composite emulsifier, methyl methacrylate, isooctyl acrylate, butyl methacrylate, acid monomers, amine monomers and crosslinking monomers, mixing in a high-pressure homogenizer for pre-emulsification, and continuously homogenizing for 40min to prepare uniform pre-emulsion.
c. Preparing a seed emulsion: adding the balance of deionized water and the balance of composite emulsifier into a reaction kettle at normal temperature and normal pressure, stirring uniformly, heating until the temperature in the kettle reaches about 80 ℃, then adding 7 percent of the total amount of the pre-emulsion into the reaction kettle, simultaneously adding the initiator solution A, controlling the temperature at about 80 ℃ and keeping the temperature for 30min to prepare the seed emulsion.
d. And d, dropwise adding the rest of pre-emulsion into the reaction kettle in the step c at a constant speed, and dropwise adding the initiator solution B into the reaction kettle at a constant speed for 3 hours.
e. And d, after the dropwise adding in the step d is finished, controlling the temperature in the reaction kettle to be about 80 ℃, and preserving the temperature for 1 h.
f. And e, cooling the reaction kettle in the step e to about 40 ℃, adding a pH regulator into the reaction kettle, regulating the pH to 8, stirring for 30min, filtering and discharging to prepare the acrylic ester microemulsion applied to the multicolor paint.
Example 4
In some embodiments, the acrylate microemulsion comprises deionized water, a composite emulsifier, methyl methacrylate, isooctyl acrylate, butyl methacrylate, an acid monomer, an amine monomer, a crosslinking monomer, an initiator and a pH regulator, wherein the components in parts by mass are respectively as follows: 100 parts of deionized water, 1 part of sodium dodecyl diphenyl ether disulfonate, 1 part of sulfosuccinic acid ethoxy ether lauryl monoester disodium salt, 1.5 parts of isomeric tridecanol polyoxyethylene ether, 1.5 parts of alkyl polyoxyethylene ether, 30 parts of methyl methacrylate, 28 parts of isooctyl acrylate, 9.3 parts of butyl methacrylate, 1.5 parts of methacrylic acid, 1.6 parts of ethylene glycol dimethacrylate, 1 part of vinyl trimethoxy silane, 0.03 part of diethyl hydroxylamine, 0.2 part of ammonium persulfate and 0.8 part of ammonia water.
Specifically, the acrylate microemulsion can be prepared by the following method:
a. preparation of initiator solution: and (2) mixing 30% of the total amount of the initiator and 3% of the total amount of the deionized water in the formula at normal temperature and normal pressure to form an initiator solution A, and then dissolving the rest of the initiator in 7% of the total amount of the deionized water to form an initiator solution B for later use.
b. Preparation of pre-emulsion: taking 40% of the total amount of the deionized water, 80% of the total amount of the composite emulsifier, methyl methacrylate, isooctyl acrylate, butyl methacrylate, acid monomers, amine monomers and crosslinking monomers, mixing in a high-pressure homogenizer for pre-emulsification, and continuously homogenizing for 40min to prepare uniform pre-emulsion.
c. Preparing a seed emulsion: adding the balance of deionized water and the balance of composite emulsifier into a reaction kettle at normal temperature and normal pressure, stirring uniformly, heating until the temperature in the kettle reaches about 82 ℃, then adding 7 percent of the total amount of the pre-emulsion into the reaction kettle, simultaneously adding the initiator solution A, controlling the temperature at about 82 ℃ and keeping the temperature for 30min to prepare the seed emulsion.
d. And d, dropwise adding the rest of pre-emulsion into the reaction kettle in the step c at a constant speed, and dropwise adding the initiator solution B into the reaction kettle at a constant speed for 3 hours.
e. And d, after the dropwise adding in the step d is finished, controlling the temperature in the reaction kettle to be about 82 ℃, and preserving the temperature for 1 h.
f. And e, cooling the reaction kettle in the step e to about 40 ℃, adding a pH regulator into the reaction kettle, regulating the pH to 8, stirring for 30min, filtering and discharging to prepare the acrylic ester microemulsion applied to the multicolor paint.
Example 5
In some embodiments, the acrylate microemulsion comprises deionized water, a composite emulsifier, methyl methacrylate, isooctyl acrylate, butyl methacrylate, an acid monomer, an amine monomer, a crosslinking monomer, an initiator and a pH regulator, wherein the components in parts by mass are respectively as follows: 100 parts of deionized water, 1 part of sulfo succinic acid ethoxy ether lauryl monoester disodium salt, 1 part of allyl ether hydroxypropyl sodium sulfonate, 1.5 parts of isomeric tridecanol polyoxyethylene ether, 1.5 parts of methallyl alcohol polyoxyethylene ether, 32 parts of methyl methacrylate, 28 parts of isooctyl acrylate, 7.3 parts of butyl methacrylate, 1 part of acrylic acid, 1.6 parts of ethylene glycol dimethacrylate, 1.2 parts of gamma-methacryloxypropyl trimethoxy silane, 0.05 part of methyldiethanolamine, 0.2 part of sodium persulfate and 1.2 parts of 2-amino-2-methyl-1-propanol.
Specifically, the acrylate microemulsion can be prepared by the following method:
a. preparation of initiator solution: and (2) mixing 30% of the total amount of the initiator and 3% of the total amount of the deionized water in the formula at normal temperature and normal pressure to form an initiator solution A, and then dissolving the rest of the initiator in 7% of the total amount of the deionized water to form an initiator solution B for later use.
b. Preparation of pre-emulsion: taking 40% of the total amount of the deionized water, 80% of the total amount of the composite emulsifier, methyl methacrylate, isooctyl acrylate, butyl methacrylate, acid monomers, amine monomers and crosslinking monomers, mixing in a high-pressure homogenizer for pre-emulsification, and continuously homogenizing for 40min to prepare uniform pre-emulsion.
c. Preparing a seed emulsion: adding the balance of deionized water and the balance of composite emulsifier into a reaction kettle at normal temperature and normal pressure, stirring uniformly, heating until the temperature in the kettle reaches about 86 ℃, then adding 7 percent of the total amount of the pre-emulsion into the reaction kettle, simultaneously adding the initiator solution A, controlling the temperature at about 86 ℃ and keeping the temperature for 30min to prepare the seed emulsion.
d. And d, dropwise adding the rest of pre-emulsion into the reaction kettle in the step c at a constant speed, and dropwise adding the initiator solution B into the reaction kettle at a constant speed for 3 hours.
e. And d, after the dropwise adding in the step d is finished, controlling the temperature in the reaction kettle to be about 86 ℃, and preserving the temperature for 1 h.
f. And e, cooling the reaction kettle in the step e to about 40 ℃, adding a pH regulator into the reaction kettle, regulating the pH to 8, stirring for 30min, filtering and discharging to prepare the acrylic ester microemulsion applied to the multicolor paint.
The final products of examples 1-5 were tested for technical specifications and compared to existing products. The test method is as follows:
method for measuring viscosity: samples were tested using a stormer viscometer at 25 ℃.
The storage stability test method comprises the following steps: after the samples were stored at 50 ℃ and 5 ℃ for 168 hours, respectively, it was observed whether there was post-thickening, delamination, or not, and if not, it was a pass.
The method for testing the high shear stability of the coating comprises the following steps: after dispersing the sample for 10min at 2000 rpm by a high-speed disperser, the sample is visually observed, and the initial state and the dispersed state of the sample are compared, wherein the smaller the difference between the initial state and the dispersed state, the better the high shear stability of the coating.
The method for testing the toughness of the color grains comprises the following steps: and after the sample is sprayed, observing whether the color grains are deformed and broken and whether the color of the color grains is clear.
TABLE 2
Referring to table 2, it can be seen that the acrylate microemulsion applied to the multicolor paint prepared by the present disclosure has superior viscosity, storage stability, particle toughness (color particle toughness) and high shear stability to the existing products.
Although the present invention has been described in detail with respect to the exemplary embodiments and advantages thereof, it should be understood that various changes, substitutions, and alterations can be made hereto without departing from the spirit and scope of the invention as defined by the appended claims. For other examples, one of ordinary skill in the art will readily appreciate that the order of the process steps may be varied while maintaining the scope of the present invention.
Moreover, the scope of the present application is not intended to be limited to the particular embodiments of the process, machine, manufacture, composition of matter, means, methods and steps described in the specification. As one of ordinary skill in the art will readily appreciate from the disclosure of the present invention, processes, machines, manufacture, compositions of matter, means, methods, or steps, presently existing or later to be developed, that perform substantially the same function or achieve substantially the same result as the corresponding embodiments described herein may be utilized according to the present invention. Accordingly, the appended claims are intended to include within their scope such processes, machines, manufacture, compositions of matter, means, methods, or steps.
Claims (10)
1. The preparation method of the acrylic ester microemulsion is characterized by comprising the following steps:
a. preparing an initiator solution: mixing 20-40% of the total amount of the initiator and 3% of the total amount of the deionized water at normal temperature and normal pressure to form an initiator solution A; mixing 7% of the total amount of the deionized water with the rest of the initiator to form an initiator solution B for later use;
b. preparing a pre-emulsion: mixing 30-40% of deionized water, 70-80% of composite emulsifier, methyl methacrylate, isooctyl acrylate, butyl methacrylate, acid monomer, amine monomer and crosslinking monomer in a high-pressure homogenizer, pre-emulsifying, and homogenizing for 40min to obtain pre-emulsion;
c. preparing a seed emulsion: adding the balance of deionized water and the balance of composite emulsifier into a reaction kettle at normal temperature and normal pressure, uniformly stirring, raising the temperature in the kettle to be more than or equal to 78 ℃, then adding 5-10% of the total amount of the pre-emulsion into the reaction kettle, simultaneously adding an initiator solution A, controlling the temperature to be 80-86 ℃ and keeping the temperature for 30min to prepare the seed emulsion;
d. c, dropwise adding the rest of pre-emulsion into the reaction kettle in the step c at a constant speed, and simultaneously dropwise adding an initiator solution B into the reaction kettle at a constant speed for 2-3 h;
e. after the dropwise adding in the step d is finished, controlling the temperature in the reaction kettle to be 80-86 ℃, and preserving the heat for 1-2 hours;
f. and e, cooling the reaction kettle in the step e to be less than or equal to 40 ℃, adding a pH regulator into the reaction kettle, regulating the pH to be 7-9, stirring for 30min, filtering and discharging to prepare the acrylate microemulsion applied to the multicolor paint.
2. The preparation method according to claim 1, wherein the composite emulsifier comprises an anionic emulsifier and a nonionic emulsifier, and the mass ratio of the anionic emulsifier to the nonionic emulsifier is 1: 1 to 3.
3. The preparation method according to claim 2, wherein the anionic emulsifier is one or more of sodium dodecyl diphenyl ether disulfonate, disodium lauryl monoester sulfosuccinate ethoxylate, sodium allyl ether hydroxypropyl sulfonate, and the like, and is mixed in any proportion.
4. The preparation method of claim 3, wherein the nonionic emulsifier is one of or a mixture of isomeric tridecanol polyoxyethylene ether, alkyl polyoxyethylene ether and methallyl alcohol polyoxyethylene ether in any proportion.
5. The method according to claim 4, wherein the acid monomer is one of acrylic acid and methacrylic acid or a mixture thereof at an arbitrary ratio.
6. The method according to claim 5, wherein the amine monomer is one or more of diethylaniline, diethylhydroxylamine, and methyldiethanolamine.
7. The method according to claim 6, wherein the crosslinking monomer is one or more of allyl methacrylate, ethylene glycol dimethacrylate, vinyltrimethoxysilane and gamma-methacryloxypropyltrimethoxysilane, and the components are mixed in any proportion.
8. The preparation method according to claim 7, wherein the initiator is one or more of ammonium persulfate, potassium persulfate and sodium persulfate, and the components are mixed in any proportion.
9. The method according to claim 6, wherein the pH adjusting agent is one of ammonia water and 2-amino-2-methyl-1-propanol or a mixture thereof at an arbitrary ratio.
10. The acrylic ester microemulsion is applied to a multicolor paint and is characterized by comprising the following components in parts by weight: 100 parts of deionized water, 2-8 parts of a composite emulsifier, 20-50 parts of methyl methacrylate, 20-60 parts of isooctyl acrylate, 20-50 parts of butyl methacrylate, 2-8 parts of an acid monomer, 1-3 parts of an amine monomer, 1-3 parts of a crosslinking monomer, 0.1-0.5 part of an initiator and 1-2 parts of a pH regulator;
the acrylate microemulsion is prepared by the preparation method of any one of claims 1 to 8.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202111020810.XA CN113896827A (en) | 2021-09-01 | 2021-09-01 | Acrylate microemulsion and preparation method thereof |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202111020810.XA CN113896827A (en) | 2021-09-01 | 2021-09-01 | Acrylate microemulsion and preparation method thereof |
Publications (1)
Publication Number | Publication Date |
---|---|
CN113896827A true CN113896827A (en) | 2022-01-07 |
Family
ID=79188298
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN202111020810.XA Pending CN113896827A (en) | 2021-09-01 | 2021-09-01 | Acrylate microemulsion and preparation method thereof |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN113896827A (en) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN115701832A (en) * | 2022-09-21 | 2023-02-14 | 张家港市德宝化工有限公司 | Preparation of metal ion dispersant by using ethylene glycol dimethacrylate wastewater |
Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN105884962A (en) * | 2014-12-31 | 2016-08-24 | 衡水新光化工有限责任公司 | Emulsion for stonelike paint and stonelike paint with emusion as film forming matter |
CN106084139A (en) * | 2016-08-16 | 2016-11-09 | 衡水新光化工有限责任公司 | The acrylic emulsion of a kind of water-soluble colorful coating and preparation technology thereof |
CN106632893A (en) * | 2016-12-31 | 2017-05-10 | 上海巴德富实业有限公司 | Acrylic acid finish emulsion and preparation method thereof |
CN107163761A (en) * | 2017-05-19 | 2017-09-15 | 佛山市顺德区巴德富实业有限公司 | A kind of colorful base paint emulsion of excellent performance and preparation method thereof |
CN109369844A (en) * | 2018-09-18 | 2019-02-22 | 佛山市顺德区巴德富实业有限公司 | A kind of pure-acrylic emulsion and preparation method thereof of super spot-resistant |
CN110330853A (en) * | 2019-07-25 | 2019-10-15 | 江苏康爱特环境工程集团有限公司 | A kind of water polyacrylic acid lotion and its preparation method and application method |
-
2021
- 2021-09-01 CN CN202111020810.XA patent/CN113896827A/en active Pending
Patent Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN105884962A (en) * | 2014-12-31 | 2016-08-24 | 衡水新光化工有限责任公司 | Emulsion for stonelike paint and stonelike paint with emusion as film forming matter |
CN106084139A (en) * | 2016-08-16 | 2016-11-09 | 衡水新光化工有限责任公司 | The acrylic emulsion of a kind of water-soluble colorful coating and preparation technology thereof |
CN106632893A (en) * | 2016-12-31 | 2017-05-10 | 上海巴德富实业有限公司 | Acrylic acid finish emulsion and preparation method thereof |
CN107163761A (en) * | 2017-05-19 | 2017-09-15 | 佛山市顺德区巴德富实业有限公司 | A kind of colorful base paint emulsion of excellent performance and preparation method thereof |
CN109369844A (en) * | 2018-09-18 | 2019-02-22 | 佛山市顺德区巴德富实业有限公司 | A kind of pure-acrylic emulsion and preparation method thereof of super spot-resistant |
CN110330853A (en) * | 2019-07-25 | 2019-10-15 | 江苏康爱特环境工程集团有限公司 | A kind of water polyacrylic acid lotion and its preparation method and application method |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN115701832A (en) * | 2022-09-21 | 2023-02-14 | 张家港市德宝化工有限公司 | Preparation of metal ion dispersant by using ethylene glycol dimethacrylate wastewater |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN108047834B (en) | Easily-oriented high-performance fluorine-silicon composite water-based aluminum powder paint and preparation method thereof | |
DE102006050336A1 (en) | Gemini surfactant-containing dispersion powder compositions | |
DE102007033596A1 (en) | Coatings with high weathering resistance, process for their preparation and their use | |
EP0623659A2 (en) | Use of a multi-staged latex and a process for making the multi-staged latex | |
DE102004057996A1 (en) | Hydrophobic additive | |
DE102005012986A1 (en) | Dispersion composition for highly flexible, waterproof, hydraulically setting tile adhesives | |
CN105037648A (en) | Slump-retaining water-reducing polycarboxylic acid water reducing agent and low-temperature quick preparation method thereof | |
CN104419272B (en) | Prepare the method for transparent/translucent colored dispersion and by its obtained colored dispersion | |
WO2013093632A2 (en) | Polymer dispersions, their preparation and use | |
JP2010522798A (en) | Acrylic ester copolymer composition and redispersible powder | |
CN108424487A (en) | A kind of organic-silicon-modified emulsion water-proof agent of desulfurated plaster and preparation method thereof | |
CN106830749A (en) | A kind of color liquid sliver and preparation method thereof | |
CN102224207A (en) | Resin emulsion for sealer | |
CN106478861A (en) | A kind of modified aqueous acrylic acid resin and the method preparing manually color sand using it | |
CN113896827A (en) | Acrylate microemulsion and preparation method thereof | |
EP2812291A1 (en) | Aqueous dispersion | |
KR102058176B1 (en) | Aqueous acrylic emulsion resin and method for preparing the same | |
US4409355A (en) | Process for preparing high solids copolymer latices with low viscosity | |
CN103232566B (en) | Preparation method of high-solid-content low-viscosity acrylate emulsion for sealing gum | |
CN109265625B (en) | Acrylic emulsion special for real stone paint and preparation method and application thereof | |
CN112300318B (en) | Environment-friendly room-temperature self-crosslinking acrylate emulsion, preparation method and application thereof | |
CN113929825A (en) | Carboxylic styrene-butadiene latex for building coating and preparation method thereof | |
CN111826052B (en) | Organic-inorganic nano hybrid water-based anti-blocking paint special for excavator bucket teeth and preparation method thereof | |
CN108395784A (en) | A kind of preparation method and product of suitable baking high-performance water-based damping coating material | |
CN107641402B (en) | Nano flame-retardant stone paint and preparation method thereof |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PB01 | Publication | ||
PB01 | Publication | ||
SE01 | Entry into force of request for substantive examination | ||
SE01 | Entry into force of request for substantive examination |