KR102207356B1 - Manufacturing method for fine particles of zinc phosphate having a plate shape by chemical method - Google Patents

Abstract

The application technology of the present application reduces the concentration of reactants of zinc salts and phosphate salts to provide inorganic precipitates of zinc phosphate in the process of manufacturing a zinc phosphate-based water-dispersible surface conditioner, which is a chemical conversion agent. When mixing and providing zinc phosphate-based inorganic precipitates, small particulate matter at the level of pulverization is produced, so even if the pulverization step is not provided or minimized, it is possible to provide a zinc phosphate-based surface conditioner composition having excellent dispersibility in water. It is an invention completed by confirming that it can be
The present application provides a method for manufacturing plate-shaped zinc phosphate fine particles by chemical method to strengthen the foundation of the ever-evolving metal surface treatment field. The plate-shaped zinc phosphate fine particles are used to prepare a water-dispersible zinc phosphate-based surface modifier. In the manufacturing method, the step of preparing a source of zinc salts and phosphate salts; Dilution step of low concentration of zinc salt and phosphate; Mixing the diluted zinc salt and phosphate; Filtering step; Washing step; It is a technology related to the scientific manufacturing method of plate-shaped zinc phosphate fine particles including a drying step.

Description

Manufacturing method for fine particles of zinc phosphate having a plate shape by chemical method}

The present invention relates to a method for manufacturing plate-shaped zinc phosphate fine particles by a chemical method, and more particularly, a step of preparing a source of zinc salts and phosphate salts; Dilution step of low concentration zinc salt and phosphate; Mixing the diluted zinc salt and phosphate; Filtering step; Washing step; It is a technology related to the method of manufacturing plate-shaped zinc phosphate fine particles to eliminate or minimize the pulverization process of particles during the manufacturing process of the zinc phosphate-based water-dispersible surface conditioner including the drying step.

Metal corrosion is a phenomenon that chemically reacts with the environment surrounding the metal and dissolves or changes to rust, and a part of it is lost, resulting in the destruction of the metal and shortening the useful life of the metal. And various methods for improving the functionality of the surface are being sought, and surface treatment technology is being developed by mobilizing knowledge.

Among them, phosphate coating treatment is one of the chemical conversion treatment methods of steel or aluminum. It is a technology that chemically reacts metal with dilute phosphoric acid to form a layer of phosphate or oxide film with high fixability and stability. It is a reaction that causes corrosion to metal by using chemical properties, and chemical process treatment of metal surface such as pretreatment of paint, wear resistance, lubrication of plastic deformation processing, electrical insulation and corrosion resistance by providing metal protection as well as functionality of the metal surface It can be called a construction method.

The phosphate film formation mechanism proceeds as shown in Reaction Formulas 1 to 4 below, and the main components are Me(H ₂ PO ₄ ) ₂ , H ₃ PO ₄ , and NO ₃ , NO ₂ , -ClO ₃ , -BrO ₃ , H ₂ O _2, etc. are used as accelerators.

Fe + 2H ₂ PO ₄ → Fe(2H ₂ PO ₄ ) ₂ + H ₂ ↑--------------------<Scheme 1>

Me + 2H ₂ PO ₄ → Me(2H ₂ PO ₄ ) ₂ + H ₂ ↑

3Me(2H ₂ PO ₄ ) ₂ ↔ Me(PO ₄ ) ₂ + 4H ₂ PO ₄ --------------------<Scheme 2> 2Me(2H ₂ PO ₄ ) ₂ + Fe(H ₂ PO ₄ ) ₂ + 4H ₂ O →MeFe(PO ₄ ) ₂ 4H ₂ O (main component of the film, Phosphophylite) + 4H ₂ PO ₄ ------------ ----------------------<Scheme 3>

3Me(H ₂ PO ₄ ) ₂ 4H ₂ O → Me ₂ (PO ₄ ) ₂ H ₂ O (main component of the film, Phosphophylite) + 4H ₂ PO ₄ -------------- --------------------------------------<Scheme 4>

When phosphoric acid is supplied to the metal surface as in Scheme 1, iron phosphate and zinc phosphate are generated as in Scheme 2, and phosphoric acid is dissociated at the same time, thereby forming insoluble tribasic zinc phosphate crystals as in Scheme 3.

At this time, the first zinc phosphate [Zn(H ₂ PO ₄ ) ₂ ] in the treatment solution is decomposed to form a film of the formula (2), and free phosphoric acid consumed in the reaction (1) is recovered.

Surface modifier is an activation process that accelerates the film through a dense and fast reaction.After phosphate film, the surface is treated with a surface modifier before phosphate film treatment to prevent defects such as bad cratering, orange peeling, metalli mark, blistering, peeling, and rust in the painting. In addition, it is necessary to supply various types of surface modifiers more suitable according to each process condition so as to have the ability of a chemical conversion film to have the ability of a chemical conversion film, centering on the colloidal particles on the seed present in the surface steel sheet.

Automobile parts are subjected to surface conditioning treatment using a phosphate coating control agent to improve corrosion resistance and promote reaction before phosphate coating treatment, as well as to provide a uniform coating treatment, and zinc phosphate-based surface adjusters widely used in the phosphate coating field until now. Since the powdery titanium series is used, the working environment can be deteriorated by dust during the working process, and it can cause respiratory disease of the worker, as well as the additional work process, resulting in lower productivity, and it is made of powder. As a result, the specific surface area due to coarsening of the particles is relatively low, and the function of the surface modifier cannot be fully exhibited. Therefore, it is inevitable that expensive multinational companies import and use water-dispersible liquid surface modifiers.

In order to manufacture a liquid surface conditioner with excellent physical properties for phosphate coating treatment, the most important factor is to make the crystal of the phosphate coating dense, to minimize the size of the particles, to shorten the coating time as much as possible, as well as to environmental pollution. In order to prevent and secure price competitiveness, it is necessary to reduce the consumption of chemicals, and a surface modifier having long-term durability is required.

However, in the case of surface conditioning agents that have been produced, sold, and used so far, due to lack of technology, the size of the surface conditioning agent particles is minimized through a grinding process that is required for a long time. It is economically difficult to put into the process by installing a large, expensive wet grinder (Pin mill, Ball mill, Attrition mill, etc.) to produce a surface modifier with excellent physical properties, and to secure price and technical competitiveness. In order to produce a beautiful surface conditioner for the purpose, the manufacturing process is simple and it is necessary to minimize expensive equipment. For this purpose, the particle shape and size of the surface conditioner material Size control is required.

No matter what physical method powder materials are pulverized, there is a great limitation in manufacturing nano-sized particles of a micrometer size or less.In particular, surface control agents at home and abroad that have been researched and developed so far are expensive due to the need for a pulverization process that relies on huge equipment. It increases the economic burden of the enterprise due to the purchase of the pulverizer, and the cost competitiveness of the product and the technology competitiveness of the enterprise are greatly reduced as a long time is required by the crushing process of the surface conditioner material.

Therefore, in order to provide a liquid water-dispersible zinc phosphate-based surface conditioner, a solution of diluted zinc salt and phosphate is added dropwise while stirring at high speed while keeping the concentration of zinc salts and phosphate salts low. Because plate-like particles of zinc phosphate precipitates are formed, a pulverization process is not required or minimized, and a zinc phosphate-based surface modifier having excellent dispersing power in water can be manufactured.Therefore, a pulverization process is required for water dispersion of conventional inorganic particles. Economic, temporal, and technical problems can be largely solved.

Looking at the technology for pulverizing inorganic substances in the prior art, Korean Patent Laid-Open Publication No. 10-2018-0119126 A shows that even when an inorganic filler having a small average particle diameter or a large specific surface area is used, the fine circuit formation ability is excellent and the dielectric loss tangent is low. A resin composition capable of obtaining a cargo has been proposed.In this cited invention, in order to constitute an inorganic material having a small average particle diameter or a large surface area so as to constitute a resin composition in which the inorganic filler is uniformly dispersed in water, a grinding process must be performed. This is a technology that has the disadvantage of not only increasing the economic burden of the company for purchasing expensive crushing equipment, but also taking a long time for crushing, which greatly reduces workability.

However, in the present application, when the concentration of the reactant for providing the inorganic precipitate is mixed in a low state and reacted, small particles of a pulverization level are generated, so that a composition having excellent dispersibility in water can be provided without providing a pulverization step. Accordingly, it can be said that the inventive concept is higher than that of the cited invention.

In Korean Patent Laid-Open Publication No. 10-2015-0136135 A, a chemical conversion treatment agent that can impart excellent corrosion resistance and moisture resistance to aluminum-based metal materials, excellent adhesion to the laminate film, excellent hydrofluoric acid resistance, and alkali resistance. And a water-dispersible chemical treatment agent that is not layered and uniformly dispersed because it contains one or more metal elements (A) selected from the group consisting of zirconium, titanium and hafnium, and vanadium element (B). In order to provide this, it is necessary to minimize the particle size of metal elements with a large specific gravity, so the pulverization process for this is indispensable, adding to the economic burden of purchasing huge expensive pulverizing equipment and taking time for the crushing process. While it is a technology that has a problem of lowering price competitiveness due to lowering properties, in the present application, when the concentration of the reactant to provide inorganic precipitates is mixed at a low concentration and precipitated, and the reactant is provided, a small particulate matter with a pulverization level is generated. Since the composition having excellent dispersibility in water can be provided without providing a pulverization step, the inventive concept may be more advanced than the cited invention.

In Korea Laid-Open Patent Publication No. 10-2014-0106938 A, 2 to 10% by weight of a phosphoric acid compound, 0.5 to 3% by weight of a manganese ion compound, 0.1 to 1% by weight of a zirconium compound, 1 to 4% by weight of an inorganic metal sol, and a vanadium compound A chemical conversion treatment composition for magnesium containing 0.05 to 1% by weight and an extra water-soluble solvent and a surface treatment method of magnesium and magnesium alloy materials using the same are provided. In the above invention, an inorganic metal sol is used to constitute a conversion treatment composition for magnesium. As (sol) is used, in order to uniformly disperse metals and insoluble inorganic substances with a high specific gravity including particulate matter in water, even if a dispersant and other additives are included in the water, the particulate matter must have a large specific gravity. The pulverization process is necessary for this, as it is possible only when the size of the particle is small, whereas in the present application, the concentration of the reactant to provide the inorganic precipitate required for the final target is mixed at a low concentration to precipitate, and when the reactant is provided, it is pulverized. It can be said that the present technology is more advanced than the cited invention, as it has a great advantage of providing a composition having excellent dispersibility in water even if it does not provide a pulverization step or minimizes it because a small particulate matter of a level is produced.

The insoluble components of the target object required for the chemical conversion treatment agent to prevent metal corrosion should be maintained in high quality, and even after a long period of time, the layer should not be separated in the water-dispersed state, and should be kept in a uniform state, but the insoluble components provided by the prior art have specific gravity. Because of its very large size, even if the dispersion technology is excellent, it must be composed of small particles less than a micrometer size in order to uniformly disperse in water for a long period of time, and this requires the purchase of expensive crushing equipment as the crushing process must be accompanied. There has been a problem that the price competitiveness due to the burden of labor costs may be lowered because time and manpower were required not only due to the additional crushing process, but also a solution to the problem has been required.

In this application, in the process of manufacturing a zinc phosphate-based water-dispersible surface modifier, a chemical conversion agent, in order to provide an inorganic precipitate of zinc phosphate, the concentration of reactants of zinc salts and phosphate salts is mixed in a low state. In the case of providing zinc phosphate-based inorganic precipitates, it is possible to provide a zinc phosphate-based surface modifier composition having a plate-like structure excellent in dispersibility in water even when the pulverization step is not provided or minimized because small particulate matter of the pulverization level is generated. As a confirmed and completed invention, the present application provides a method for manufacturing plate-shaped zinc phosphate fine particles by a chemical method, thereby reinforcing the base of the ever-evolving metal surface treatment field and creating an item according to a new new technology.

The technical idea of the present application presented as a means for achieving the above object is a technique related to the chemical manufacturing method of plate-shaped zinc phosphate fine particles for obtaining a plate-shaped zinc phosphate fine particle by a chemical method for preparing a water-dispersible zinc phosphate-based surface modifier, zinc salt (Zinc salts) and phosphate (Phosphate salts) source (Source) preparation step of the first step; A second step of diluting the zinc salt and phosphate concentration to a concentration range of 0.01 to 1.5% by weight in order not to pulverize or to minimize the pulverization process and to provide a plate-shaped zinc phosphate-based fine particle; A third step of mixing the diluted zinc salt and phosphate produced in the dilution step of the second step to obtain insoluble plate-shaped zinc phosphate fine particles; A configuration comprising a fourth step of filtering, washing, and drying a solution containing plate-shaped zinc phosphate precipitates obtained through the third step and accompanying by-products to obtain powdery zinc phosphate-based precipitates with no residual by-products. It is an invention of the technical idea to achieve the object of the present application with a method for producing chemical plate-shaped zinc phosphate fine particles characterized by.

Hereinafter, the technical idea of the present application will be described in detail.

In the first step of the present application, in the step of preparing the source of zinc salts and phosphate salts, the steps of preparing the source of zinc salts include zinc oxide, zinc sulfate, and At least one zinc salt selected from zinc chloride, zinc nitrate, zinc hydroxide, and zinc acetate is dissolved in water or diluted inorganic acid, As shown in Chemical Reaction Formula 5, carbon dioxide (CO2) gas, sodium carbonate, sodium bicarbonate, potassium carbonate, potassium bicarbonate, ammonium carbonate, ammonium bicarbonate ), supply at least one carbonate selected in the range above the stoichiometric value of the zinc salt so that zinc carbonate is formed.

ZnSO ₄ + (NH ₄ ) ₂ CO ₃ -> ZnCO ₃ + (NH ₃ ) ₂ SO ₄ ------<Scheme 5>

In the case of the source preparation step of the phosphate salts, Phosphoric acid or sodium phosphate, monosodium phosphate, dibasic sodium phosphate, potassium phosphate, monobasic potassium phosphate, dibasic potassium phosphate, ammonium phosphate , Ammonium monophosphate and ammonium dibasic phosphate may be selected from at least one phosphate.

The dilution step of low concentration zinc salt and phosphate in the second process is a process aimed at providing zinc phosphate-based fine particles having a plate structure while not grinding or minimizing the grinding process. In the step, each zinc salt and phosphate concentration can be diluted to a concentration of 0.01 to 1.5% by weight, preferably 0.1 to 1.25% by weight, and more preferably, it is advantageous to be diluted to 0.25 to 1.0% by weight. And, most preferably, it is advantageous to be diluted with 0.5 to 0.75% by weight.When each zinc salt and phosphate concentration is diluted to 0.01% by weight or less, plate-shaped fine phosphoric acid in the mixing step of the diluted zinc salt and phosphate below It can have a great advantage of providing sufficient dispersing power to prepare a water-dispersible zinc phosphate-based surface modifier because it can precipitate zinc-based inorganic substances, but the amount of zinc phosphate-based precipitates is small, so productivity is lowered as well as particle size is reduced. Since it is very low, there may be a problem that a lot of processing and time are required in the filtration and water washing steps in the following steps.If the concentration of each zinc salt and phosphate is diluted to 1.5% by weight or more, the following diluted zinc salt and phosphate are mixed. Depending on the steps, a large amount of plate-shaped zinc phosphate precipitate can be made, but if the concentration of the diluted solid content is high, the particle size of the plate-shaped zinc phosphate-based precipitate can be enlarged and the specific gravity of the unit precipitate can be increased. However, it is preferable to select the dilution ratio of the proposed concentration, as the problem of layer separation is provided.

The third step, the mixing step of diluted zinc salt and phosphate, aims to provide insoluble plate-shaped zinc phosphate fine particles as shown in Scheme 6 by mixing each diluted zinc salt and phosphate produced by the dilution step. In the mixing step of the diluted zinc salt and phosphate, it is preferable to stir at a speed of 150 to 300 rpm or higher in order to obtain a plate acid-type zinc phosphate-based precipitate of a uniform size to obtain an optimal particle size.

ZnCO ₃ + 2H ₃ PO ₄ -> ZnPO ₄ + 3H ₂ O + CO ₂ -------------<Scheme 6>

The third process, the filtering step, the water washing step, and the drying step, are not particularly limited, and a solution containing a plate-shaped zinc phosphate precipitate produced by the mixing step of the diluted zinc salt and phosphate and accompanying by-products is filtered, As long as the powdery zinc phosphate-based precipitates with no residual by-products can be obtained by separating, all are possible without limitation.

Hereinafter, embodiments in which the technical idea of the present application is implemented will be described in detail together with examples of the invention in the specific content section for carrying out the following invention.

As discussed above, in order to disperse the insoluble component of the target object required for chemical treatment in water so far, if the size of the insoluble particles is large or the specific gravity is large, the dispersion may not be performed, and the layer separation may result in a significant decrease in marketability. Therefore, in order to overcome this problem, it must be pulverized to a size less than that capable of providing dispersion power.

In order to provide a water-dispersible composition with excellent dispersing power without layer separation for insoluble, high specific gravity inorganic substances, a pulverization process through a pulverizer is essential, which increases the economic burden of companies required to purchase expensive pulverization equipment, as well as pulverization. It is a situation that requires a lot of time and manpower required for the process.

In this application, a source of zinc salts and phosphate salts is prepared to solve the problem of the conventional method, which requires a pulverization process due to lack of technology so far in order to disperse the target insoluble component in water. step; Dilution step of low concentration of zinc salt and phosphate; Mixing the diluted zinc salt and phosphate; Filtering step; Washing step; As we have secured the technology to produce zincation with minimized particle size and flake type only by chemical treatment including the drying step, there have been various kinds of surface conditioning agents for phosphate coating treatment. It is effective in maximizing the activity of the surface treatment modifier while overcoming the problem of.

Figure 1: Process chart for the method for manufacturing plate-shaped zinc phosphate fine particles by the chemical method of the present invention
Figure 2: EDS (Energy Dispersive Spectrometer) analysis result of the plate-shaped zinc phosphate precipitate obtained by the embodiment of the present invention
Figure 3: XRD (X-ray Powder Diffraction) analysis result of the plate-shaped zinc phosphate precipitate obtained by the embodiment of the present invention
Figure 4: SEM (Scanning Electron Microscope) analysis result of the plate-shaped zinc phosphate precipitate obtained by the embodiment of the present invention
Figure 5: Dispersion test results of a zinc phosphate-based water-dispersible surface modifier for a plate-shaped zinc phosphate-based precipitate obtained by an example of the present invention

Prior to describing the embodiments of the invention for implementing the technical idea of the present application as examples, terms or words used in the specification or claims of the present application shall not be construed as being limited to a conventional or dictionary meaning, The scope of protection of the present application should be interpreted as a meaning and concept consistent with the technical idea of the present invention, and the examples described in this specification are only the most preferred embodiment of the present invention and do not represent all the technical ideas of the present application. However, it should be understood that there may be various equivalents and modified examples that can replace them at the time of application.

1 is a diagram showing a process chart for a method for manufacturing plate-shaped zinc phosphate fine particles by a chemical method according to the technical idea of the present invention. In FIG. 1, the preparation step of the source of zinc salts and phosphate salts is It is the part described as the first step in the means of solving the problem, the dilution step to obtain a low concentration of zinc salt and phosphate is described as the second step, and the step of mixing the diluted zinc salt and phosphate is described as the third step. And, it is described as a fourth process including filtration, washing and drying processes.

Hereinafter, an example in which the technical idea of the present application is applied by the following inventive examples will be described in detail as a means for specifying and describing embodiments in which the present invention is implemented.

Example 1

After dissolving the zinc chloride (ZnCl ₂ ) of Samjeon Pure Chemical in a 1 liter beaker, a precipitate of zinc carbonate was prepared as a zinc-based source while stirring this solution and purging carbon dioxide (CO ₂ ) gas.

After supplying 0.1 g of the prepared zinc carbonate precipitate to a 1 liter beaker, while stirring at 500 rpm using a mechanical stirrer, 1/100 diluted phosphoric acid (H ₃ PO ₄ ) was slowly added dropwise thereto, followed by about 20 minutes. After maintaining the state to prepare zinc phosphate fine particles having a plate-like structure, the particles were filtered and washed three times, and then heated and dried in an oven at 100°C.

Example 2

After dissolving the zinc nitrate (ZnNO ₃ ·6H ₂ O) of Samjeon Pure Chemical in a 1 liter beaker, a precipitate of zinc carbonate was prepared as a zinc-based source by purging carbon dioxide (CO ₂ ) gas while stirring the solution. .

After supplying 0.5 g of the prepared zinc carbonate precipitate to a 1 liter beaker, 1/100 diluted phosphoric acid (H ₃ PO ₄ ) was slowly added dropwise while stirring at 500 rpm using a mechanical stirrer. After maintaining the state to prepare zinc phosphate fine particles having a plate-like structure, the particles were filtered and washed three times, and then heated and dried in an oven at 100°C.

Example 3

After measuring 10 g of zinc hydroxide (Zn(OH) ₂ ) of Samjeon Pure Chemical in a 1 liter beaker, supply diluted hydrochloric acid to 1/5, and then heat, dissolve, and cool on a hot plate. While stirring, sodium carbonate (Na ₂ CO ₃ ) solution diluted to 1/5 was slowly added dropwise to prepare a precipitate of zinc carbonate.

After supplying 1.5 g of the prepared zinc carbonate precipitate to a 1 liter beaker, while stirring at 500 rpm using a mechanical stirrer, 1/5 diluted sodium phosphate (NaH ₂ PO ₄ ) was slowly added dropwise and about After maintaining the state for 20 minutes to prepare zinc phosphate fine particles having a plate-like structure, the particles were filtered and washed three times, and then heated and dried in an oven at 100°C.

Comparative Examples 1 to 3

It was carried out in the same manner as in Examples 1 to 3, except that 10 g of the precipitates of zinc carbonate prepared in Examples 1 to 3 were supplied.

To check the average particle size and dispersion power of the zinc phosphate-based precipitates prepared in Comparative Examples 1 to 3 and Examples 1 to 3, the average particle size was confirmed by a Mastersizer 3000 E laser diffraction particle size analyzer, Dispersing power is 3.3% by weight of Sannov Korea dispersant (SN disoers), 3.0% by weight of wetting agent (Koremul NP-8), 2.0% by weight of antifoaming agent (Sannov Korea), 1.0 to 100% by weight of the prepared zinc phosphate precipitate. After measuring weight% of thickener (methyl cellulose) and 80% by weight of distilled water in a basket mill, a 1 mm zirconia ceramic ball was stirred and dispersed at a speed of 1,000 rpm, and this solution was mixed with a 100 ml measuring cylinder. After the (Mass cylinder) fractionation, the time at which the layer separation starts was checked, and the test results are shown in Table 1.

division Average particle size
(㎛) Delamination time Example 1 0.48 Not observed after 7 days Example 2 0.52 Not observed after 7 days Example 3 0.64 Not observed after 7 days Comparative Example 1 23 2.5 hours Comparative Example 2 28 1.5 hours Comparative Example 3 25 2 hours

As shown in Table 1 above, in Comparative Examples 1 to 3, a large amount of zinc phosphate was provided when a high concentration aqueous solution of zinc salt and phosphate was provided during the process of preparing zinc phosphate-based precipitates and then mixed during the agitating process of the solution. Precipitates may be formed, but as the size of the particles appears to be 23 micrometers or more and the layer is separated within 2 hours and 30 minutes, the pulverization process by a grinder is required to manufacture the zinc phosphate-based water-dispersible surface regulator. Was confirmed.

On the other hand, in Examples 1 to 3, when an aqueous solution of a low concentration of zinc salt and phosphate was provided during the process of preparing a zinc phosphate-based precipitate, and when the solution was mixed during the stirring process, the particle size was about 0.5 microns. In addition, as the dispersion power through this example is excellent and there is no possibility of layer separation within one week, there is no need for a grinding process to prepare a water-dispersible surface control agent for the zinc phosphate-based precipitate obtained according to the present application. Confirmed.

Therefore, in manufacturing the zinc phosphate-based surface conditioning agent according to the present application, economic feasibility and technological prowess can be secured, which is expected to greatly contribute to the creation of technological prowess and economic benefits of enterprises.

Figure 2 shows the EDS (Energy Dispersive Spectrometer) analysis results of the plate-shaped zinc phosphate precipitate obtained by the examples of the present invention, which is to confirm the presence of ZnPO ₄ and other components to be obtained from the present application. Qualitative analysis experimental data, Figure 3 shows the XRD (X-ray Powder Diffraction) analysis results of the plate-shaped zinc phosphate precipitate obtained by the embodiment of the present invention, which is an experiment to confirm the crystal structure of the precipitate 4 shows the results of SEM (Scanning Electron Microscope) analysis of the plate-shaped zinc phosphate precipitate obtained according to the embodiment of the present invention. Magnification of the precipitates photographed at different angles by magnifying with an electron microscope Photographs are shown in 4a and 4b, and FIG. 5 is a result of a dispersion test of a zinc phosphate-based water-dispersible surface conditioner for a plate-shaped zinc phosphate-based precipitate obtained according to an embodiment of the present invention. As a result of confirming whether or not the precipitate obtained in this application can maintain a high dispersing power, it was confirmed that the resultant fine particles obtained by the inventor's intention maintains a high dispersing power for a long time.

FIG. 1 shows a process chart for a method for manufacturing plate-shaped zinc phosphate fine particles by the chemical method of the present invention, and FIG. 2 is an EDS (Energy Dispersive Spectrometer) analysis of plate-shaped zinc phosphate-based precipitates obtained by an embodiment of the present invention. 3 is an X-ray Powder Diffraction (XRD) analysis result of a plate-shaped zinc phosphate precipitate obtained by an example of the present invention, and FIG. 4 is a plate-shaped obtained by an example of the present invention. Is the SEM (Scanning Electron Microscope) analysis result of the zinc phosphate-based precipitate of, and FIG. 5 is a dispersion test result of a zinc phosphate-based water-dispersible surface conditioner for the plate-shaped zinc phosphate-based precipitate obtained by an embodiment of the present invention. As shown, a separate code description is not required.

Claims (4)

In the chemical manufacturing method of plate-shaped zinc phosphate fine particles by obtaining plate-shaped zinc phosphate fine particles by a chemical method for preparing a water-dispersible zinc phosphate-based surface modifier,
In the first step of preparing the source of zinc salts and phosphate salts, the source of zinc salts is zinc oxide, zinc sulfate, and chloride. A pretreatment step of dissolving a zinc salt selected from zinc chloride, zinc nitrate, zinc hydroxide, and zinc acetate with water or diluted inorganic acid, and
Carbon dioxide (CO ₂ ) gas, sodium carbonate, sodium bicarbonate, potassium carbonate, potassium bicarbonate, ammonium carbonate, ammonium bicarbonate A source of zinc salts is prepared by supplying carbonates above the stoichiometric value of zinc salts that have gone through the pretreatment step to obtain zinc carbonate.
Phosphate salts Source is Phosphoric acid, sodium phosphate, monosodium phosphate, dibasic sodium, potassium phosphate, monobasic potassium, dibasic potassium, ammonium phosphate, monobasic ammonium phosphate, A first process in which a phosphate salt selected from diammonium phosphate is prepared as a source of phosphate salts;
A second step of diluting the zinc salt and phosphate concentration to a concentration range of 0.01 to 1.5% by weight in order not to pulverize or to minimize the pulverization process and to provide a plate-shaped zinc phosphate-based fine particle;
A third step of mixing the diluted zinc salt and phosphate produced in the dilution step of the second step to obtain insoluble plate-shaped zinc phosphate fine particles;
A fourth step of filtering, washing, and drying a solution containing the plate-like zinc phosphate precipitate obtained through the third step and the accompanying by-products to obtain a powdery zinc phosphate-based precipitate without remaining by-products;
Plate-shaped zinc phosphate fine particles manufacturing method by a chemical method comprising a. delete delete The method of claim 1,
Plate-shaped phosphoric acid according to a chemical method, characterized in that it is applied to stir at a speed in the range of 150 to 300 rpm in order to obtain a precipitate of plate-shaped zinc phosphate having a uniform size in the mixing step of the diluted zinc salt and phosphate in the third step. Zinc fine particles manufacturing method.

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