CN112552708A - Dispersible barium sulfate composite powder for water-based paint and preparation method thereof - Google Patents
Dispersible barium sulfate composite powder for water-based paint and preparation method thereof Download PDFInfo
- Publication number
- CN112552708A CN112552708A CN202011493728.4A CN202011493728A CN112552708A CN 112552708 A CN112552708 A CN 112552708A CN 202011493728 A CN202011493728 A CN 202011493728A CN 112552708 A CN112552708 A CN 112552708A
- Authority
- CN
- China
- Prior art keywords
- barium sulfate
- composite powder
- melamine resin
- water
- melamine
- 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.)
- Withdrawn
Links
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/10—Treatment with macromolecular organic compounds
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/02—Compounds of alkaline earth metals or magnesium
- C09C1/027—Barium sulfates
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/006—Combinations of treatments provided for in groups C09C3/04 - C09C3/12
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/04—Physical treatment, e.g. grinding, treatment with ultrasonic vibrations
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/08—Treatment with low-molecular-weight non-polymer organic compounds
-
- 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
- C09D5/1687—Use of special additives
-
- 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
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
- C09D7/62—Additives non-macromolecular inorganic modified by treatment with other compounds
-
- 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
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/63—Additives non-macromolecular organic
-
- 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
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/65—Additives macromolecular
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Inorganic Chemistry (AREA)
- Paints Or Removers (AREA)
Abstract
The invention belongs to the technical field of coatings, and provides dispersible barium sulfate composite powder for a water-based coating and a preparation method thereof. The composite powder can improve the compatibility and the dispersibility of the barium sulfate powder in the paint, can effectively prevent the barium sulfate from settling, endows the paint with higher hardness, mechanical strength and gloss, enhances the light resistance and the stain resistance of the paint, and can further improve the dispersion and suspension characteristics of the powder in the water-based paint.
Description
Technical Field
The invention relates to the technical field of coatings, in particular to dispersible barium sulfate composite powder for a water-based coating and a preparation method thereof.
Background
Barium sulfate is used as pigment and filler of paint and plays an important role in improving the thickness, wear resistance, water resistance, acid and alkali resistance, heat resistance, surface hardness, impact resistance and the like of paint.
The high-gloss barium sulfate is a barite raw ore and is processed by the processes of ore dressing, ore washing, crushing and the like. Moderate hardness, brittleness, stable chemical property, insolubility in water, ethanol and hydrochloric acid, acid and alkali resistance, water resistance, etc. The white pigment has the characteristics of high whiteness and good leveling property, is an effective and cheap white material, and can replace 10-25% of the titanium dioxide in the water-based paint.
The high-gloss barium sulfate has the advantages of strong chemical inertia, good stability, acid and alkali resistance, moderate hardness, high specific gravity, high whiteness, capability of absorbing harmful rays and the like, and is widely used for various high-grade coatings. In particular, the excellent acid and alkali resistance of barium sulfate is suitable for heavy-duty anticorrosive coatings, and can be used for long-term corrosion prevention in relatively severe corrosive environments such as chemical and marine environments.
However, the high-gloss barium sulfate has a high density, and needs to be thinned to a thickness of 5 μm or less in the coating material, and thus is highly likely to cause agglomeration and sedimentation in the coating material. In particular, barium sulfate is generally used for heavy duty anticorrosive coatings, which are applied thickly, generally exceeding 300 μm, and the high density and easy agglomeration of barium sulfate causes deposition during the drying process of the coating, resulting in uneven protection of the coating.
The adoption of high-dispersion auxiliary agent is a mature technical means for processing the dispersion performance of inorganic powder at present, for example, the surface modification treatment is carried out on barium sulfate powder by using the auxiliary agent with high activity, the surface energy of the powder can be effectively reduced, the steric hindrance between particles can be increased by surfactant molecules, the particles are prevented from approaching each other, the particles are prevented from being aggregated due to collision, but the dispersion effect is limited, and particularly, the problem of sedimentation is difficult to solve by only depending on a dispersing agent for barium sulfate with high density. Thus, it is an urgent need in the coatings market to solve the problem of dispersion and settling of barium sulfate for coatings.
The invention patent CN200680046633.X discloses a technology of ultrafine barium sulfate, a water-based coating composition and a water-based ink composition, and provides that hydroxide and/or oxide of Al, Si and Zr is coated on the surface of the ultrafine barium sulfate; and/or phosphates of Mg, Ca, Sr, Ba. This technique improves the dispersibility of barium sulfate by forming an inorganic coating on the surface of barium sulfate. The invention patent CN202010536738.5 discloses a method for preparing barium sulfate for plastics and coatings, which comprises the steps of crushing barite, adding hot concentrated sulfuric acid for dissolving, adding an impurity removal reagent consisting of sodium diethyldithiocarbamate, ethylene diamine tetraacetic acid and polyacrylamide for removing impurities to obtain barium sulfate slurry; adding the barium sulfate slurry into a surface modifier, and adding a compound modifier consisting of kaolin, starch, melamine, sulfonated hydrogenated castor oil succinate and polyetherimide for modification to obtain modified barium sulfate slurry; then filter pressing is carried out by a filter press, and then drying, crushing and screening are carried out to prepare the barium sulfate powder for plastics and coatings, and the obtained barium sulfate powder has the advantages of high whiteness, high glossiness, good stability, good dispersibility, low oil absorption value, good mechanical property and processability and the like. The invention patent CN201910813187.X discloses a modification method of nano barium sulfate, which comprises the steps of adding nano barium carbonate powder into a powder modifying machine, and adding a dispersing agent consisting of sodium laureth sulfate and alkylphenol polyoxyethylene ether for modification; adding nano barium carbonate into a reaction kettle, preparing slurry, adding concentrated sulfuric acid under the stirring state, adjusting the pH to 6-7 by using sodium hydroxide to prepare barium sulfate slurry, and filtering and drying to prepare barium sulfate powder; conveying barium sulfate powder to a powder modifying machine, adding a modifying agent consisting of a rare earth coupling agent and dimethylsilyl cage-shaped polysilsesquioxane for surface modification, drying and crushing to prepare a nano barium sulfate product, wherein the dispersibility of the nano barium sulfate powder can be effectively improved, and the processing performance and the stability are improved. Although the prior art mentioned above promotes the dispersibility of barium sulfate, the barium sulfate is still inorganic, the dispersibility is limited, and the density of barium sulfate is still high, and the precipitation in the coating material is inevitable.
Disclosure of Invention
Aiming at the use problems that the existing superfine barium sulfate used for paint is easy to agglomerate, high in density and easy to settle, the invention provides the dispersible barium sulfate composite powder used for water-based paint and the preparation method thereof.
Firstly, a preparation method of dispersible barium sulfate composite powder for water-based paint is provided, which is characterized by comprising the following steps: the preparation method comprises the following steps:
(1) weighing melamine and formaldehyde according to the molar ratio of 2.2: 1; weighing ethylene glycol which is 2.5 times of the mass of the melamine; firstly, uniformly mixing formaldehyde and ethylene glycol, adding triethanolamine, adjusting the pH value to 8, adding melamine, continuously raising the temperature and stirring, controlling the temperature raising rate at 1 ℃/min, raising the temperature to 60 ℃, and then stirring at constant temperature for 15-20min to obtain pre-polymerized melamine resin solution;
(2) adding the fine barium sulfate into a high-speed mixer, and stirring at high speed by using the high-speed mixer at the constant temperature of 90 ℃ by using an oil bath to fully suspend the fine barium sulfate; then, mixing the melamine resin solution obtained in the step (1) with caprolactam according to the mass ratio of 5:1, and spraying to uniformly wrap the melamine resin solution on the surface of the superfine barium sulfate; spraying amount is 30% of the mass of the fine barium sulfate, after spraying, raising the temperature of the high-speed mixer to 150 ℃, increasing the rotating speed, further polymerizing the pre-polymerized melamine resin, performing thermal curing at high temperature, and attaching the pre-polymerized melamine resin to the interface of the fine barium sulfate to obtain the barium sulfate treated by the melamine resin;
(3) and (3) mixing the barium sulfate treated by the melamine resin obtained in the step (2), the butyl sodium naphthalene sulfonate and the sulfonated melamine formaldehyde resin according to the mass ratio of 100:0.1-0.5:0.2-0.5, and dispersing by a vortex air flow machine to obtain the dispersible barium sulfate composite powder for the water-based paint.
Preferably, the barium sulfate with the particle size less than 5 μm is selected as the fine barium sulfate in the step (2).
Preferably, the high-speed stirring in the step (2) adopts a rotation speed of 400-600rpm, and the fine barium sulfate is fully contacted with the sprayed pre-polymerized melamine resin liquid in a complete suspension state through the high-speed stirring, so that the melamine resin liquid is uniformly coated on the surface of the fine barium sulfate.
Preferably, in the step (2), the rotation speed is increased to 900-1000rpm, the pre-polymerized melamine resin is further polymerized along with the increase of the temperature, and the melamine resin is cured along with the increase of the temperature to 150 ℃, and the adhesion between powder materials during polymerization and curing is prevented by increasing the stirring speed.
Preferably, the temperature of the high-speed mixer in the step (2) is 150 ℃, and the melamine resin is fully cured by stirring at high speed for 10-15 min.
Because the melamine resin is solidified and attached to the interface of the barium sulfate in the step (2), adhesion exists, preferably, the butyl sodium naphthalene sulfonate and the sulfonated melamine formaldehyde resin are added in the step (3) for dispersion, the adhered particles are thinned and dispersed in a vortex air flow machine, and the butyl sodium naphthalene sulfonate and the sulfonated melamine formaldehyde resin are used for further dispersing the barium sulfate treated by the melamine resin; the sodium butylnaphthalenesulfonate can obviously reduce the surface tension of water, has excellent penetrability and wettability, and is beneficial to promoting the dispersion and diffusion of barium sulfate in the water-based paint; the sulfonated melamine formaldehyde resin belongs to an anionic surfactant, has suspension property on inorganic powder, is favorable for promoting barium sulfate to be compositely suspended in the coating and prevents sedimentation.
In the step (3), the rotational speed of the vortex air flow machine is controlled to be reasonable, the attached melamine resin is easy to fall off due to too high rotational speed and too strong shearing, the rotational speed is too low to refine the adhered large particles, and the rotational speed of the main machine is preferably 300-400 rpm.
In addition, the invention provides the dispersible barium sulfate composite powder for the water-based paint prepared by the method. The invention aims to improve the dispersibility of barium sulfate in the coating and prevent the barium sulfate from settling, so that the melamine resin thermosetting body is firmly attached to the interface of the barium sulfate to form the composite powder, and the density of the obtained barium sulfate composite powder is reduced without the high-density settlement of the barium sulfate. The melamine resin and the barium sulfate are compounded, so that the density of the composite powder can be reduced, the suspension property in the coating is enhanced, the compatibility of barium sulfate inorganic powder and the organic matrix of the coating can be increased, and the modified barium sulfate composite powder can be uniformly suspended and dispersed in the coating and does not settle. Meanwhile, after the melamine resin and barium sulfate composite powder is added into the coating, the melamine resin has the characteristics of high hardness, good gloss, high mechanical strength, light resistance and stain resistance, and when the barium sulfate powder after being compounded is added into the coating for coating and using, the coating can be endowed with higher hardness, mechanical strength and gloss feeling, and the light resistance and stain resistance of the coating are enhanced. In-situ polymerization of melamine resin on barium sulfate powder not only enhances the dispersibility of barium sulfate in the coating and prevents the barium sulfate from settling, but also improves a series of performances of the coating. Further, barium sulfate treated by dispersing melamine resin by using sodium butylnaphthalene sulfonate and sulfonated melamine formaldehyde resin is easy to wet and disperse in the water-based paint and suspend at the same time. The barium sulfate composite powder obtained by the invention is applied to water-based paint, and is obviously improved in the aspects of dispersibility, anti-settling property and affinity.
The remarkable advantages are that:
1. the melamine resin is firmly polymerized in situ on the barium sulfate powder and is firmly attached to a barium sulfate interface to form the composite powder, so that the density of the composite powder is reduced, the compatibility and the dispersibility of the barium sulfate powder in the coating are improved, and the barium sulfate can be effectively prevented from settling.
2. The melamine resin composite barium sulfate powder can endow the paint with higher hardness, mechanical strength and gloss feeling, and enhance the light resistance and stain resistance of the paint.
3. The sodium butylnaphthalenesulfonate and the sulfonated melamine formaldehyde resin can further improve the dispersion and suspension characteristics of the powder in the water-based paint, and further improve the anti-settling effect of the powder.
Drawings
FIG. 1 is a photograph of barium sulfate composite powder prepared in example 1 of the present invention, taken by scanning electron microscope at 3000 times;
FIG. 2 is a photograph of barium sulfate composite powder prepared in example 1 of the present invention, taken by scanning electron microscope at 5000X;
FIG. 3 is a 50000 times scanning electron microscope photograph of the barium sulfate composite powder prepared in example 1 of the present invention;
FIG. 4 is a photograph of a sample of barium sulfate composite powder prepared in example 1 of the present invention, which was left standing for 24 hours in a paint, without generating sedimentation;
FIG. 5 is a photograph of a sample of the barium sulfate composite powder prepared in comparative example 1, which was left standing for 24 hours in a paint, with barium sulfate completely settled;
FIG. 6 is a photograph of a sample of the barium sulfate composite powder prepared in comparative example 2, which was left standing for 24 hours in a paint, without generation of sedimentation;
FIG. 7 is a photograph of a sample of the barium sulfate composite powder prepared in comparative example 3, which was left standing for 24 hours in a paint, showing little sedimentation.
Detailed Description
The present invention will be described in further detail with reference to specific embodiments, but it should not be construed that the scope of the present invention is limited to the following examples. Various substitutions and alterations can be made by those skilled in the art and by conventional means without departing from the spirit of the method of the invention described above.
Example 1
Weighing melamine and formaldehyde according to the molar ratio of 2.2: 1; weighing ethylene glycol which is 2.5 times of the mass of the melamine; first, uniformly mixing formaldehyde and ethylene glycol, adding triethanolamine, adjusting the pH value to 8, adding melamine, continuously raising the temperature and stirring, controlling the temperature raising rate at 1 ℃/min, raising the temperature to 60 ℃, and then stirring at constant temperature for 15min to obtain the pre-polymerized melamine resin solution. Adding the fine barium sulfate with the particle size of less than 5 microns into a high-speed mixer, and stirring the fine barium sulfate at a high speed of 400rpm by using the high-speed mixer at a constant temperature of 90 ℃ by using an oil bath to fully suspend the fine barium sulfate; then, mixing the pre-polymerized melamine resin liquid with caprolactam according to the mass ratio of 5:1, and spraying to uniformly wrap the melamine resin liquid on the surface of the superfine barium sulfate; and the spraying amount is 30% of the mass of the fine barium sulfate, after the spraying is finished, the temperature of the high-speed mixer is increased to 150 ℃, the rotating speed is increased to 900rpm, the high-speed stirring is carried out for 10min, the pre-polymerized melamine resin is further polymerized, the pre-polymerized melamine resin is thermally cured at high temperature, and the pre-polymerized melamine resin is attached to the interface of the fine barium sulfate to obtain the barium sulfate treated by the melamine resin. Mixing barium sulfate treated by melamine resin, sodium butylnaphthalene sulfonate and sulfonated melamine formaldehyde resin according to the mass ratio of 100:0.1:0.2, and dispersing by a vortex air flow machine to obtain the dispersible barium sulfate composite powder for the water-based paint, wherein the rotating speed of a host machine of the vortex air flow machine is 300 rpm.
Example 2
Weighing melamine and formaldehyde according to the molar ratio of 2.2: 1; weighing ethylene glycol which is 2.5 times of the mass of the melamine; firstly, uniformly mixing formaldehyde and ethylene glycol, adding triethanolamine, adjusting the pH value to 8, adding melamine, continuously raising the temperature and stirring, controlling the temperature raising rate at 1 ℃/min, raising the temperature to 60 ℃, and then stirring at constant temperature for 16min to obtain the pre-polymerized melamine resin solution. Adding the fine barium sulfate with the particle size of less than 5 microns into a high-speed mixer, and stirring the fine barium sulfate at a high speed of 500rpm by using the high-speed mixer at a constant temperature of 90 ℃ by using an oil bath to fully suspend the fine barium sulfate; then, mixing the pre-polymerized melamine resin liquid with caprolactam according to the mass ratio of 5:1, and spraying to uniformly wrap the melamine resin liquid on the surface of the superfine barium sulfate; and the spraying amount is 30% of the mass of the fine barium sulfate, after the spraying is finished, the temperature of the high-speed mixer is increased to 150 ℃, the rotating speed is increased to 900rpm, the high-speed stirring is carried out for 12min, the pre-polymerized melamine resin is further polymerized, the pre-polymerized melamine resin is thermally cured at high temperature, and the pre-polymerized melamine resin is attached to the interface of the fine barium sulfate to obtain the barium sulfate treated by the melamine resin. Mixing barium sulfate treated by melamine resin, sodium butylnaphthalene sulfonate and sulfonated melamine formaldehyde resin according to the mass ratio of 100:0.2:0.2, and dispersing by a vortex air flow machine to obtain the dispersible barium sulfate composite powder for the water-based paint, wherein the rotating speed of a host machine of the vortex air flow machine is 300 rpm.
Example 3
Weighing melamine and formaldehyde according to the molar ratio of 2.2: 1; weighing ethylene glycol which is 2.5 times of the mass of the melamine; first, uniformly mixing formaldehyde and ethylene glycol, adding triethanolamine, adjusting the pH value to 8, adding melamine, continuously raising the temperature and stirring, controlling the temperature raising rate at 1 ℃/min, raising the temperature to 60 ℃, and then stirring at constant temperature for 18min to obtain the pre-polymerized melamine resin solution. Adding the fine barium sulfate with the particle size of less than 5 microns into a high-speed mixer, and stirring the fine barium sulfate at a high speed of 500rpm by using the high-speed mixer at a constant temperature of 90 ℃ by using an oil bath to fully suspend the fine barium sulfate; then, mixing the pre-polymerized melamine resin liquid with caprolactam according to the mass ratio of 5:1, and spraying to uniformly wrap the melamine resin liquid on the surface of the superfine barium sulfate; and the spraying amount is 30% of the mass of the fine barium sulfate, after the spraying is finished, the temperature of the high-speed mixer is increased to 150 ℃, the rotating speed is increased to 1000rpm, the high-speed stirring is carried out for 13min, the pre-polymerized melamine resin is further polymerized, the pre-polymerized melamine resin is thermally cured at high temperature, and the pre-polymerized melamine resin is attached to the interface of the fine barium sulfate to obtain the barium sulfate treated by the melamine resin. Mixing barium sulfate treated by melamine resin, sodium butylnaphthalene sulfonate and sulfonated melamine formaldehyde resin according to the mass ratio of 100:0.3:0.3, and dispersing by a vortex air flow machine to obtain the dispersible barium sulfate composite powder for the water-based paint, wherein the rotating speed of a host machine of the vortex air flow machine is 350 rpm.
Example 4
Weighing melamine and formaldehyde according to the molar ratio of 2.2: 1; weighing ethylene glycol which is 2.5 times of the mass of the melamine; first, uniformly mixing formaldehyde and ethylene glycol, adding triethanolamine, adjusting the pH value to 8, adding melamine, continuously raising the temperature and stirring, controlling the temperature raising rate at 1 ℃/min, raising the temperature to 60 ℃, and then stirring at constant temperature for 19min to obtain the pre-polymerized melamine resin solution. Adding the fine barium sulfate with the particle size of less than 5 microns into a high-speed mixer, and stirring the fine barium sulfate at a high speed of 500rpm by using the high-speed mixer at a constant temperature of 90 ℃ by using an oil bath to fully suspend the fine barium sulfate; then, mixing the pre-polymerized melamine resin liquid with caprolactam according to the mass ratio of 5:1, and spraying to uniformly wrap the melamine resin liquid on the surface of the superfine barium sulfate; and the spraying amount is 30% of the mass of the fine barium sulfate, after the spraying is finished, the temperature of the high-speed mixer is increased to 150 ℃, the rotating speed is increased to 1000rpm, the high-speed stirring is carried out for 14min, the pre-polymerized melamine resin is further polymerized, the pre-polymerized melamine resin is thermally cured at high temperature, and the pre-polymerized melamine resin is attached to the interface of the fine barium sulfate to obtain the barium sulfate treated by the melamine resin. Mixing barium sulfate treated by melamine resin, sodium butylnaphthalene sulfonate and sulfonated melamine formaldehyde resin according to the mass ratio of 100:0.4:0.4, and dispersing by a vortex air flow machine to obtain the dispersible barium sulfate composite powder for the water-based paint, wherein the rotating speed of a host machine of the vortex air flow machine is 400 rpm.
Example 5
Weighing melamine and formaldehyde according to the molar ratio of 2.2: 1; weighing ethylene glycol which is 2.5 times of the mass of the melamine; firstly, uniformly mixing formaldehyde and ethylene glycol, adding triethanolamine, adjusting the pH value to 8, adding melamine, continuously raising the temperature and stirring, controlling the temperature raising rate at 1 ℃/min, raising the temperature to 60 ℃, and then stirring at constant temperature for 20min to obtain the pre-polymerized melamine resin solution. Adding the fine barium sulfate with the particle size of less than 5 microns into a high-speed mixer, and stirring the fine barium sulfate at a high speed of 600rpm by using the high-speed mixer at a constant temperature of 90 ℃ by using an oil bath to fully suspend the fine barium sulfate; then, mixing the pre-polymerized melamine resin liquid with caprolactam according to the mass ratio of 5:1, and spraying to uniformly wrap the melamine resin liquid on the surface of the superfine barium sulfate; and the spraying amount is 30% of the mass of the fine barium sulfate, after the spraying is finished, the temperature of the high-speed mixer is increased to 150 ℃, the rotating speed is increased to 1000rpm, the high-speed stirring is carried out for 15min, the pre-polymerized melamine resin is further polymerized, the pre-polymerized melamine resin is thermally cured at high temperature, and the pre-polymerized melamine resin is attached to the interface of the fine barium sulfate to obtain the barium sulfate treated by the melamine resin. Mixing barium sulfate treated by melamine resin, sodium butylnaphthalene sulfonate and sulfonated melamine formaldehyde resin according to the mass ratio of 100: 0.5: 0.5, and dispersing by a vortex air flow machine to obtain the dispersible barium sulfate composite powder for the water-based paint, wherein the rotating speed of a host machine of the vortex air flow machine is 400 rpm.
Comparative example 1
Mixing fine barium sulfate with the particle size of less than 5 mu m, sodium butylnaphthalene sulfonate and sulfonated melamine formaldehyde resin according to the mass ratio of 100:0.1:0.2, and dispersing by using a vortex air flow machine to obtain barium sulfate powder for the water-based coating, wherein the rotating speed of a host machine of the vortex air flow machine is 300 rpm.
Comparative example 2
Weighing melamine and formaldehyde according to the molar ratio of 2.2: 1; weighing ethylene glycol which is 2.5 times of the mass of the melamine; first, uniformly mixing formaldehyde and ethylene glycol, adding triethanolamine, adjusting the pH value to 8, adding melamine, continuously raising the temperature and stirring, controlling the temperature raising rate at 1 ℃/min, raising the temperature to 60 ℃, and then stirring at constant temperature for 15min to obtain the pre-polymerized melamine resin solution. Adding the fine barium sulfate with the particle size of less than 5 microns into a high-speed mixer, and stirring the fine barium sulfate at a high speed of 400rpm by using the high-speed mixer at a constant temperature of 90 ℃ by using an oil bath to fully suspend the fine barium sulfate; then, mixing the pre-polymerized melamine resin liquid with caprolactam according to the mass ratio of 5:1, and spraying to uniformly wrap the melamine resin liquid on the surface of the superfine barium sulfate; and the spraying amount is 30% of the mass of the fine barium sulfate, after the spraying is finished, the temperature of the high-speed mixer is increased to 150 ℃, the rotating speed is increased to 900rpm, the high-speed stirring is carried out for 10min, the pre-polymerized melamine resin is further polymerized, the pre-polymerized melamine resin is thermally cured at high temperature, and the pre-polymerized melamine resin is attached to the interface of the fine barium sulfate to obtain the barium sulfate treated by the melamine resin. Mixing barium sulfate treated by melamine resin and sulfonated melamine formaldehyde resin according to the mass ratio of 100:0.2, and dispersing by a vortex air flow machine to obtain the dispersible barium sulfate composite powder for the water-based paint, wherein the rotating speed of a host machine of the vortex air flow machine is 300 rpm.
Comparative example 3
Weighing melamine and formaldehyde according to the molar ratio of 2.2: 1; weighing ethylene glycol which is 2.5 times of the mass of the melamine; first, uniformly mixing formaldehyde and ethylene glycol, adding triethanolamine, adjusting the pH value to 8, adding melamine, continuously raising the temperature and stirring, controlling the temperature raising rate at 1 ℃/min, raising the temperature to 60 ℃, and then stirring at constant temperature for 15min to obtain the pre-polymerized melamine resin solution. Adding the fine barium sulfate with the particle size of less than 5 microns into a high-speed mixer, and stirring the fine barium sulfate at a high speed of 400rpm by using the high-speed mixer at a constant temperature of 90 ℃ by using an oil bath to fully suspend the fine barium sulfate; then, mixing the pre-polymerized melamine resin liquid with caprolactam according to the mass ratio of 5:1, and spraying to uniformly wrap the melamine resin liquid on the surface of the superfine barium sulfate; and the spraying amount is 30% of the mass of the fine barium sulfate, after the spraying is finished, the temperature of the high-speed mixer is increased to 150 ℃, the rotating speed is increased to 900rpm, the high-speed stirring is carried out for 10min, the pre-polymerized melamine resin is further polymerized, the pre-polymerized melamine resin is thermally cured at high temperature, and the pre-polymerized melamine resin is attached to the interface of the fine barium sulfate to obtain the barium sulfate treated by the melamine resin. Mixing barium sulfate treated by melamine resin and sodium butylnaphthalene sulfonate according to the mass ratio of 100:0.1, and dispersing by a vortex air flow machine to obtain the dispersible barium sulfate composite powder for the water-based paint, wherein the rotating speed of a host machine of the vortex air flow machine is 300 rpm.
The barium sulfate composite powder obtained in example 1 was subjected to morphology analysis. According to the general rule of TY/T010-1996 analytical scanning electron microscope method, the detection instrument is a JSM-7500 scanning electron microscope, and the test is carried out by an analytical test center of Sichuan university. As shown in fig. 1, which is a photograph of the barium sulfate composite powder prepared in example 1, taken by scanning electron microscope at 3000 times, melamine resin was adhered to the barium sulfate; further magnification to 5000 times, as in fig. 2; enlarged to 50000 times, as shown in FIG. 3, the melamine resin was adhered tightly to the barium sulfate.
150g of the samples prepared in examples 1-5 and comparative examples 1-3 are respectively weighed, and are mixed with 200g of distilled water, 10g of propylene glycol and 320g of styrene-acrylic emulsion to prepare an experimental coating, the experimental coating is uniformly stirred and then is kept stand to observe the sedimentation condition, and the settlement condition is shown in table 1.
Table 1:
| sample (I) | Standing for 6h | Standing for 12h | Standing for 24h |
| Example 1 | Without sedimentation | Without sedimentation | Without sedimentation |
| Example 2 | Without sedimentation | Without sedimentation | Without sedimentation |
| Example 3 | Without sedimentation | Without sedimentation | Without sedimentation |
| Example 4 | Without sedimentation | Without sedimentation | Without sedimentation |
| Example 5 | Without sedimentation | Without sedimentation | Without sedimentation |
| Comparative example 1 | The occurrence of sedimentation | Complete sedimentation of barium sulfate | Complete sedimentation of barium sulfate |
| Comparative example 2 | Without sedimentation | Without sedimentation | Without sedimentation |
| Comparative example 3 | Without sedimentation | Without sedimentation | The occurrence of sedimentation |
After the sample prepared according to the preparation method in the embodiment is added into the coating taking the styrene-acrylic emulsion as the matrix, the suspension performance is good, and the barium sulfate composite powder can be placed for a long time without sedimentation, for example, fig. 4 shows a picture of the sample of the barium sulfate composite powder prepared in the embodiment 1 when the barium sulfate composite powder is used in the coating and is kept still for 24 hours, and no sedimentation occurs; in comparative example 1, the barium sulfate is not cured and attached by melamine resin, the obtained barium sulfate powder has high density and is easy to settle when being used for coating, and for example, as shown in fig. 5, the barium sulfate composite powder prepared in comparative example 1 is used for a sample photo of standing in the coating for 24 hours, and the barium sulfate is completely settled; in the comparative example 2, when the barium sulfate treated by the melamine resin is refined and dispersed in a vortex air flow machine, no sodium butylnaphthalenesulfonate is added, so that the barium sulfate is poor in wettability and slow in dispersion when used for a water-based paint, but has an excellent anti-settling effect, and as shown in fig. 6, the barium sulfate composite powder prepared in the comparative example 2 is used for a sample photo of standing for 24 hours in the paint, no settlement is generated; in the comparative example 3, the barium sulfate treated by the melamine resin is not added with the sulfonated melamine formaldehyde resin when being refined and dispersed in a vortex air flow machine, and the suspension property is influenced to a certain extent when the barium sulfate is used for a water-based paint, for example, a sample photo that the barium sulfate composite powder prepared in the comparative example 3 is used for standing for 24 hours in the paint appears a little sedimentation in fig. 7.
Claims (9)
1. A preparation method of dispersible barium sulfate composite powder for water-based paint is characterized by comprising the following steps:
(1) weighing melamine, formaldehyde and ethylene glycol, firstly, uniformly mixing the formaldehyde and the ethylene glycol, adding triethanolamine, adjusting the pH value to 8, adding the melamine, continuously raising the temperature and stirring, controlling the temperature raising rate at 1 ℃/min, raising the temperature to 60 ℃, and then stirring at constant temperature for 15-20min to obtain pre-polymerized melamine resin solution;
(2) adding the fine barium sulfate into a high-speed mixer, and stirring at high speed by using the high-speed mixer at the constant temperature of 90 ℃ by using an oil bath to fully suspend the fine barium sulfate; then, mixing the melamine resin solution obtained in the step (1) with caprolactam according to the mass ratio of 5:1, and spraying to uniformly wrap the melamine resin solution on the surface of the superfine barium sulfate; spraying amount is 30% of the mass of the fine barium sulfate, after spraying, raising the temperature of the high-speed mixer to 150 ℃, increasing the rotating speed, further polymerizing the pre-polymerized melamine resin, performing thermal curing at high temperature, and attaching the pre-polymerized melamine resin to the interface of the fine barium sulfate to obtain the barium sulfate treated by the melamine resin;
(3) and (3) mixing the barium sulfate treated by the melamine resin obtained in the step (2), sodium butylnaphthalene sulfonate and sulfonated melamine formaldehyde resin according to a certain mass ratio, and dispersing by a vortex air flow machine to obtain the dispersible barium sulfate composite powder for the water-based paint.
2. The method for preparing the dispersible barium sulfate composite powder for the water-based paint according to claim 1, characterized in that: in the step (1), melamine and formaldehyde are weighed according to the molar ratio of 2.2: 1; ethylene glycol was weighed to be 2.5 times the mass of melamine.
3. The method for preparing the dispersible barium sulfate composite powder for the water-based paint according to claim 1, characterized in that: in the step (2), the superfine barium sulfate is barium sulfate with the particle size of less than 5 mu m.
4. The method for preparing the dispersible barium sulfate composite powder for the water-based paint according to claim 1, characterized in that: in the step (2), the high-speed stirring adopts the rotation speed of 400-600 rpm.
5. The method for preparing the dispersible barium sulfate composite powder for the water-based paint according to claim 1, characterized in that: in the step (2), the rotation speed is increased to 900-.
6. The method for preparing the dispersible barium sulfate composite powder for the water-based paint according to claim 1, characterized in that: and (3) in the step (2), the temperature of the high-speed mixer is 150 ℃, and the high-speed stirring is carried out for 10-15min at the temperature.
7. The method for preparing the dispersible barium sulfate composite powder for the water-based paint according to claim 1, characterized in that: in the step (3), barium sulfate treated by melamine resin, sodium butylnaphthalene sulfonate and sulfonated melamine formaldehyde resin are mixed according to the mass ratio of 100:0.1-0.5: 0.2-0.5.
8. The method for preparing the dispersible barium sulfate composite powder for the water-based paint according to claim 1, characterized in that: in step (3), the host machine speed of the vortex air flow machine is 300-400 rpm.
9. A dispersible barium sulfate composite powder for water-based paint is characterized in that: prepared by the preparation method of any one of claims 1 to 8.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011493728.4A CN112552708A (en) | 2020-12-17 | 2020-12-17 | Dispersible barium sulfate composite powder for water-based paint and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011493728.4A CN112552708A (en) | 2020-12-17 | 2020-12-17 | Dispersible barium sulfate composite powder for water-based paint and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN112552708A true CN112552708A (en) | 2021-03-26 |
Family
ID=75064468
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202011493728.4A Withdrawn CN112552708A (en) | 2020-12-17 | 2020-12-17 | Dispersible barium sulfate composite powder for water-based paint and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112552708A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113429808A (en) * | 2021-06-28 | 2021-09-24 | 成都新柯力化工科技有限公司 | Isolation dispersant for preventing graphene agglomeration, preparation method and application method |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3318714A (en) * | 1965-10-23 | 1967-05-09 | Eastman Kodak Co | Pigment dispersions |
| US5427854A (en) * | 1994-03-14 | 1995-06-27 | E. I. Du Pont De Nemours And Company | Fibers containing polymer-coated inorganic particles |
| CA2453887A1 (en) * | 2002-12-20 | 2004-06-20 | Frank Schilke | Bone cement having improved mechanical properties, and process for the preparation thereof |
| CN109971039A (en) * | 2019-04-09 | 2019-07-05 | 东北林业大学 | A kind of preparation method of modified melamine-formaldehyde resin encapsulated red phosphorus |
-
2020
- 2020-12-17 CN CN202011493728.4A patent/CN112552708A/en not_active Withdrawn
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3318714A (en) * | 1965-10-23 | 1967-05-09 | Eastman Kodak Co | Pigment dispersions |
| US5427854A (en) * | 1994-03-14 | 1995-06-27 | E. I. Du Pont De Nemours And Company | Fibers containing polymer-coated inorganic particles |
| CA2453887A1 (en) * | 2002-12-20 | 2004-06-20 | Frank Schilke | Bone cement having improved mechanical properties, and process for the preparation thereof |
| CN109971039A (en) * | 2019-04-09 | 2019-07-05 | 东北林业大学 | A kind of preparation method of modified melamine-formaldehyde resin encapsulated red phosphorus |
Non-Patent Citations (2)
| Title |
|---|
| 原燃料化学工业部涂料技术训练班组织编: "《涂料工艺第2分册》", 31 July 1981, 石油化学工业出版社 * |
| 顾继友: "《胶粘剂与涂料》", 31 May 1999, 北京：中国林业出版社 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113429808A (en) * | 2021-06-28 | 2021-09-24 | 成都新柯力化工科技有限公司 | Isolation dispersant for preventing graphene agglomeration, preparation method and application method |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CA2347547C (en) | Processes for preparing precipitated calcium carbonate compositions and products thereof | |
| CN100447314C (en) | Titanium white for dry acrylic spinning delustering its preparing method | |
| EP0573150B1 (en) | Pigmentary material | |
| EP0359385B1 (en) | Dry ground/wet ground calcium carbonate filler compositions | |
| CN101372527B (en) | Nano-zinc oxide/acrylic ester grafting composite emulsion and preparation thereof | |
| US4898620A (en) | Dry ground/wet ground calcium carbonate filler compositions | |
| US6569920B1 (en) | Titanium dioxide slurries having improved stability | |
| CA2218287A1 (en) | Process for preparing an improved low-dusting, free-flowing pigment | |
| CN1439451A (en) | Nano-diamond deagglomeration and grading method | |
| CN110713820B (en) | Preparation method of hydrophobic modified diamond abrasive | |
| CN108751204A (en) | A kind of preparation method of submicron silicon dioxide dispersion liquid | |
| CN112552708A (en) | Dispersible barium sulfate composite powder for water-based paint and preparation method thereof | |
| CN108410017A (en) | A kind of preparation method for the high-dispersion barium sulfate composite material in plastic matrix | |
| CN101891972A (en) | Method for producing chemical fiber titanium dioxide by surface coating of common titanium dioxide (TiO2) in solvent phase | |
| US5746819A (en) | High solids anatase TiO2 slurries | |
| US3838085A (en) | Pigmented asbestos latex emulsion paint composition | |
| US5338354A (en) | Composite pigmentary material | |
| US3947286A (en) | Pigmented asbestos coating systems | |
| CN111454447A (en) | Method for dispersing nylon uvioresistant nano titanium dioxide | |
| CN111484756A (en) | Method for improving dispersion stability of alumina-coated titanium dioxide | |
| CN111574853A (en) | Modified barium sulfate for heavy-duty anticorrosive paint | |
| AU630348B2 (en) | Micro composite systems and processes for making same | |
| JP5548195B2 (en) | Method for producing barium sulfate having good dispersibility and good storage stability | |
| CN115044263A (en) | Photoaging-resistant hydroxyl acrylic resin coating and preparation method thereof | |
| CN104927399A (en) | Corrosion resistant modified calcium carbonate with excellent overall performances 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 | ||
| WW01 | Invention patent application withdrawn after publication |
Application publication date: 20210326 |
|
| WW01 | Invention patent application withdrawn after publication |