CN114773891A - Coated modified zinc powder and preparation method thereof - Google Patents

Coated modified zinc powder and preparation method thereof Download PDF

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CN114773891A
CN114773891A CN202210481592.8A CN202210481592A CN114773891A CN 114773891 A CN114773891 A CN 114773891A CN 202210481592 A CN202210481592 A CN 202210481592A CN 114773891 A CN114773891 A CN 114773891A
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zinc
zinc powder
coated modified
reaction
preparation
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CN114773891B (en
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廖有为
姜孟超
廖建春
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Hunan Jinpan New Material Technology Co ltd
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Hunan Jinpan New Material Technology Co ltd
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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/08—Anti-corrosive paints
    • C09D5/10—Anti-corrosive paints containing metal dust
    • C09D5/106—Anti-corrosive paints containing metal dust containing Zn
    • 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

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  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)

Abstract

The invention discloses coated modified zinc powder and a preparation method thereof, wherein the coated modified zinc powder is prepared by coating a nano zinc oxide film with the granularity of 1000-2000 meshes, and the thickness of the nano zinc oxide film is 10-30 nm. The invention can reduce the activation energy when the zinc powder is contacted with a corrosive medium in a large area, reduce the excessive activation of the zinc powder at the initial stage of corrosion prevention, simultaneously does not weaken the conductive capability of the zinc powder, and can enhance the weather resistance and the salt spray resistance of the zinc-rich coating; the preparation method is simple and low in cost.

Description

Coated modified zinc powder and preparation method thereof
Technical Field
The invention relates to zinc powder and a preparation method thereof, in particular to modified zinc powder and a preparation method thereof.
Background
Zinc powder is one of the most commonly used fillers in primer coatings in the field of steel corrosion protection. Primers containing zinc powder are generally referred to as zinc rich primers. The zinc-rich primer mainly depends on two means of shielding protection and cathodic protection in the process of carrying out corrosion prevention on steel. The shielding protection is to isolate the corrosive medium and the steel substrate from each other through the compactness of the coating. The cathodic protection depends on mutual contact of zinc particles and zinc particles, and zinc particles and the steel substrate in the coating of the zinc-rich primer to form a smooth conductive network, so that the aim of electrochemical protection is fulfilled. Thus, zinc powder is one of the most important fillers affecting the performance of zinc rich primers.
Research now indicates that a significant portion of the zinc in the zinc rich primer is wasted through excessive activation when the coating is exposed to a corrosive medium over a large area. This activation period usually lasts about 300 hours in a 5% NaCl solution, and during this period, the zinc powder of the coating is rapidly oxidized, so that the service life of the coating is not always equal to the theoretical value.
Disclosure of Invention
The technical problem to be solved by the invention is to overcome the defects in the prior art and provide a coated modified zinc powder and a preparation method thereof, the coated modified zinc powder can reduce the excessive activation of the zinc powder at the initial stage of corrosion prevention, does not weaken the conductive capability of the zinc powder, enhances the corrosion prevention capability of a zinc-rich coating,
the technical scheme adopted by the invention for solving the technical problems is as follows: the coated modified zinc powder is prepared by coating a nano zinc oxide film with the granularity of 1000-2000 meshes, and the thickness of the nano zinc oxide film is 10-30 nm.
The preparation method of the coated modified zinc powder comprises the following steps:
(1) respectively preparing a zinc ion solution and a urea solution;
(2) adding a surfactant into the urea solution, uniformly mixing, slowly adding the zinc ion solution while stirring, continuously stirring, and heating for reaction;
(3) adding zinc powder, vacuumizing the reaction system, stirring, heating for reaction, and separating out a precipitate part from a reaction product to obtain a precursor;
(4) and calcining the precursor under a vacuum condition, and cooling to obtain the catalyst.
Preferably, in step (1), the zinc ion solution is an inorganic zinc salt solution soluble in water.
Preferably, in the step (1), the mass ratio of zinc ions to water in the zinc ion solution is 1.8-3.5: 10-15.
Preferably, in the step (1), the mass ratio of urea to water in the urea solution is 2-3: 10-15.
More preferably, in the step (1), the solute of the zinc ion solution is one or more of zinc nitrate, zinc sulfate and zinc chloride.
Preferably, in the step (2), the surfactant is a surfactant with an HLB value of 12-15. The surfactant acts to prevent Zn (OH)2Nucleation by itself, when Zn (OH)2The surfactant also acts to prevent particle agglomeration when zinc powder is used as a nucleus to form a precipitate and grow.
Preferably, in the step (2), the mass ratio of the urea to the surfactant is 2-3: 0.2-1; the mass ratio of the urea to the zinc ions added into the reaction system is 2-3: 1.8-3.5.
More preferably, in the step (2), the surfactant is one or more than two of OP-10, OE-20 and OE-10.
Preferably, in step (2), the stirring speed is 300-500 r/min.
Preferably, in step (2), the slow addition refers to: the zinc ion solution is gradually added after 5-10 min.
Preferably, in the step (2), the temperature is increased to 80-95 ℃ for reaction; the reaction time is 30-60 min.
Preferably, in the step (3), the mass ratio of the zinc powder to the zinc ions added in the step (2) is 10-15: 1.
Preferably, in the step (3), the particle size of the zinc powder is 1000-2000 meshes.
Preferably, in the step (3), the degree of vacuum in the reaction system during the reaction is 10-3~10-5Pa。
Preferably, in the step (3), the stirring speed is 600-800 r/min. If the speed is too slow, the zinc powder is not uniformly dispersed, and if the speed is too fast, Zn (OH)2The coating was incomplete.
Preferably, in the step (3), the temperature is increased to 95-120 ℃ for reaction; the reaction time is 2-3 h.
Preferably, in the step (4), the calcining temperature is 300-400 ℃, and the calcining time is 2-3 h.
The principle of the preparation method of the invention is as follows:
in the preparation process of the invention, zinc ions and urea are mixed in the aqueous solution environment in the step (2), and the mixture is heated and stirred; at this time, urea is gradually hydrolyzed by the temperature rise to provide OH-；Zn2-With OH-Can generate water-insoluble Zn (OH)2However, this process is slow, so that there is not much Zn (OH) in the system2(ii) a In the step (3), a vacuumizing device is started to prevent the reaction of the zinc powder with oxygen and water, the hydrolysis speed of the urea can be improved by raising the temperature, and Zn (OH) in the system2Is produced in large quantities and is nucleated with zinc dust to form Zn (OH)2Coating insoluble precipitate of zinc powder; and (4) calcining the precursor under a vacuum condition. Zn (OH)2Decomposed into ZnO and H at high temperature2And O, because the water does not react with the zinc in the vacuum environment, the zinc powder coated by the nano zinc oxide is obtained after cooling.
The maximum thickness of the zinc oxide shell can be controlled by the content of urea and zinc-containing inorganic salt, and the hydrolysis degree of urea can be controlled by the reaction conditions in the steps (2) and (3), so that the thickness and the appearance of the zinc oxide shell can be further adjusted, a layer of nano zinc oxide is coated on the surface of the zinc powder, the problem that the electrical connection of the zinc powder in the coating is reduced when the thickness of the zinc oxide shell is too large is avoided, and incomplete coating caused by too small thickness of the zinc oxide shell is avoided.
The invention has the beneficial effects that: the invention can reduce the activation energy when the zinc powder is contacted with a corrosive medium in a large area, reduce the excessive activation of the zinc powder at the initial stage of corrosion prevention, simultaneously does not weaken the conductive capability of the zinc powder, and can enhance the weather resistance and the salt spray resistance of the zinc-rich coating; the preparation method is simple and low in cost.
Drawings
FIG. 1 is a scanning electron micrograph of a coated modified zinc powder of example 1 of the present invention.
FIG. 2 is a graph showing the results of a surface resistance test of a zinc-rich coating prepared using the coated modified zinc powder of example 1 of this invention.
Fig. 3 is a graph showing the results of a surface resistance test of a conventional zinc-rich coating.
FIG. 4 is a polarization curve of a zinc-rich coating prepared with the coated modified zinc powder of example 1 of this invention versus a conventional zinc-rich coating.
Fig. 5 is an optical photograph of a 1000h neutral salt spray test of a zinc-rich coating prepared using the coated modified zinc powder of example 1 of this invention.
Fig. 6 is an optical photograph of a conventional zinc-rich coating after a 1000h neutral salt spray test.
Detailed Description
The present invention will be further described with reference to the following examples and the accompanying drawings.
The starting materials used in the examples of the present invention were all obtained from conventional commercial sources.
Example 1
The coated modified zinc powder is prepared by coating a nano zinc oxide film with the granularity of 1200 meshes and the thickness of the nano zinc oxide film being 10 nm. FIG. 1 is a scanning electron micrograph of the coated modified zinc powder of this example, and it can be seen from FIG. 1 that the zinc powder is coated with a zinc oxide shell layer having a thickness of 10 nm.
The preparation method of the embodiment is as follows:
(1) preparing 4g of urea and 21g of deionized water into a urea solution, and preparing 5g of zinc nitrate (containing 3.45g of zinc ions) and 20g of deionized water into a zinc ion solution;
(2) adding 0.5g of surfactant OP-10 into the urea solution, and after uniformly stirring, putting the urea solution containing the surfactant into a three-neck flask; connecting the three-neck flask with a heating device and a vacuumizing device; starting a stirrer at a rotating speed of 300r/min, and slowly adding the zinc ion solution (the adding process takes 5 min); starting the heating device, continuing stirring, and heating to 80 ℃. Keeping the reaction for 30min for reaction;
(3) 49.5g of zinc powder (1200 mesh) was added to a three-necked flask, and the flask was evacuatedDevice, pumping to pressure of 10-3Pa; increasing the stirring speed to 600r/min, heating to 105 ℃ and reacting for 3 h; filtering the suspension obtained by the reaction, respectively washing the obtained mixture for 3 times by using deionized water and ethanol, and drying in vacuum to obtain a precursor;
(4) and (3) putting the precursor into a vacuum tube furnace, calcining for 3h at 320 ℃, cooling and taking out to obtain a final product.
The surface resistivity of the coating surface is measured by using a heavy hammer type surface resistance tester, firstly, the surface to be measured is cleaned before measurement, the heavy hammer is flatly placed on a test sample plate, and a test button is pressed until the reading is stable. The environment for each measurement was carried out in a laboratory at 25 ℃ and 60% humidity. Fig. 2 is a test result of a zinc-rich coating prepared by using the coated modified zinc powder of this embodiment, and fig. 3 is a test result of a common zinc-rich coating prepared by using common zinc powder (the content of the zinc powder in the two coatings is 95% of the solid content of the dry film, and the other components are the same), it can be seen that the surface resistivity of the zinc-rich coating prepared by using the coated modified zinc powder is consistent with that of the common zinc-rich coating, which indicates that the conductivity of the zinc-rich coating prepared by using the coated modified zinc powder of the present invention is not impaired.
Electrochemical testing was performed using an Interface1000 electrochemical workstation from Gamry electrochemical instruments, usa. The test system is a three-electrode system, a metal platinum sheet is used as an auxiliary electrode, a saturated calomel electrode is used as a reference electrode, and the reference electrode is coated with 2cm2The substrate of the zinc-rich coating was the working electrode and 3.5% NaCl solution was used as the etching medium. Fig. 4 is a polarization curve of a zinc-rich coating prepared by coating the modified zinc powder and a common zinc-rich coating (the content of the zinc powder in the two coatings is 95% of the solid content of the dry film, and the other components are the same), wherein a black line is the zinc-rich coating prepared by the modified zinc powder, and a gray line is the zinc-rich coating prepared by the common zinc powder. The absence of wave troughs in the anode curve of the black line in the figure, which represents the absence of activation-passivation of the coating, illustrates that the modified zinc powder of the invention effectively solves the problem of over-activation of the zinc powder.
The zinc-rich coating prepared by using the coated modified zinc powder of the embodiment and a normal zinc-rich coating prepared by using normal zinc powder are subjected to a neutral salt spray test for 1000h, wherein the content of the zinc powder in the two coatings is 95 percent of the solid content of a dry film, and the rest components are the same. As a result of the tests shown in FIGS. 5 and 6, it can be seen that the zinc-rich paint film of FIG. 5 is intact, whereas the zinc-rich paint film of FIG. 6 has been corroded and red rust occurs; the coated modified zinc powder greatly prolongs the cathode protection time of the coating, and the activation energy of the zinc powder is reduced.
Example 2
The coated modified zinc powder is prepared by coating a nano zinc oxide film with the granularity of 1000 meshes and the thickness of the nano zinc oxide film being 15 nm.
The preparation method of this example is as follows:
(1) preparing 6g of urea and 24g of deionized water into a urea solution, and preparing 8g of zinc chloride (containing zinc ions, 3.84 g) and 22g of deionized water into a zinc ion solution;
(2) adding 0.5g of surfactant OE-20 into the urea solution, and after uniformly stirring, putting the urea solution containing the surfactant into a three-neck flask; connecting the three-mouth flask with a heating device and a vacuumizing device; starting a stirrer, wherein the rotating speed is 500r/min, and slowly adding the zinc ion solution (the adding process takes 8 min); starting a heating device, continuously stirring, heating to 90 ℃, and keeping for 30min for reaction;
(3) 39.5g of zinc powder (1000 mesh) was added to a three-necked flask, and a vacuum-pumping apparatus was started to pump the mixture to a gas pressure of 10-3Pa; raising the stirring speed to 800r/min, raising the temperature to 105 ℃ and reacting for 2 h; filtering the suspension obtained by the reaction, respectively washing the obtained mixture for 3 times by using deionized water and ethanol, and drying in vacuum to obtain a precursor;
(4) and (3) putting the precursor into a vacuum tube furnace, calcining for 3h at 320 ℃, cooling and taking out to obtain a final product.
Example 3
The coated modified zinc powder is prepared by coating a nano zinc oxide film with the particle size of 1500 meshes and the thickness of the nano zinc oxide film being 10 nm.
The preparation method of the embodiment is as follows:
(1) preparing urea solution by 3.5g of urea and 24g of deionized water, and preparing zinc ion solution by 4g of zinc chloride (containing 1.92g of zinc ions) and 22g of deionized water;
(2) adding 0.5g of surfactant OE-20 into the urea solution, and after uniformly stirring, putting the urea solution containing the surfactant into a three-neck flask; connecting the three-neck flask with a heating device and a vacuumizing device; starting a stirrer, wherein the rotating speed is 450r/min, and slowly adding the zinc ion solution (the adding process takes 10 min); starting a heating device, continuously stirring, heating to 80 ℃, and keeping for 40min for reaction;
(3) adding 10g of zinc powder (1500 meshes) into a three-neck flask, starting a vacuum extractor, and extracting until the air pressure is 10-3Pa; raising the stirring speed to 800r/min, raising the temperature to 105 ℃ and reacting for 2 h; filtering the suspension obtained by the reaction, respectively washing the obtained mixture for 3 times by using deionized water and ethanol, and drying in vacuum to obtain a precursor;
(4) putting the precursor into a vacuum tube furnace, calcining for 3 hours at 320 ℃, cooling and taking out to obtain a final product
The above embodiments are only for illustrating the invention and are not to be construed as limiting the invention, and those skilled in the art can make various changes and modifications without departing from the spirit and scope of the invention, therefore, all equivalent technical solutions also belong to the scope of the invention, and the scope of the invention is defined by the claims.

Claims (10)

1. The coated modified zinc powder is characterized in that a nano zinc oxide film is coated with the modified zinc powder, the granularity of the zinc powder is 1000-2000 meshes, and the thickness of the nano zinc oxide film is 10-30 nm.
2. The process for the preparation of a coated modified zinc powder according to claim 1, comprising the steps of:
(1) respectively preparing a zinc ion solution and a urea solution;
(2) adding a surfactant into the urea solution, uniformly mixing, slowly adding the zinc ion solution while stirring, continuously stirring, and heating for reaction;
(3) adding zinc powder, vacuumizing the reaction system, stirring, heating for reaction, and separating a precipitate part from a reaction product to obtain a precursor;
(4) and calcining the precursor under a vacuum condition, and cooling to obtain the catalyst.
3. The method for preparing a coated modified zinc powder as defined in claim 2, wherein in step (1), the zinc ion solution is a water-soluble inorganic zinc salt solution; the mass ratio of zinc ions to water in the zinc ion solution is 1.8-3.5: 10-15; the mass ratio of urea to water in the urea solution is 2-3: 10-15.
4. The method for preparing coated modified zinc powder according to claim 3, wherein in step (1), the solute of zinc ion solution is one or more of zinc nitrate, zinc sulfate and zinc chloride.
5. The method for preparing a coated modified zinc powder according to any one of claims 2 to 4, wherein in the step (2), the surfactant is a surfactant with an HLB value of 12 to 15; the mass ratio of the urea to the surfactant is 2-3: 0.2-1; the mass ratio of the urea to the zinc ions added into the reaction system is 2-3: 1.8-3.5.
6. The method for preparing coated modified zinc powder as defined in claim 5, wherein in step (2), said surfactant is one or more of OP-10, OE-20 and OE-10.
7. The preparation method of the coated modified zinc powder as defined in any one of claims 2-6, wherein in step (2), the stirring speed is 300-500 r/min; the slow addition refers to: gradually adding zinc ion solution for 5-10 min; in the step (2), heating to 80-95 ℃ for reaction; the reaction time is 30-60 min.
8. The preparation method of the coated modified zinc powder as defined in any one of claims 2 to 7, wherein in the step (3), the mass ratio of the zinc powder to the zinc ions added in the step (2) is 10-15: 1; the particle size of the zinc powder is 1000-2000 meshes.
9. The preparation method of coated modified zinc powder as defined in any one of claims 2 to 8, wherein in the step (3), the degree of vacuum in the reaction system during the reaction process is 10-3~10-5Pa; in the step (3), the stirring speed is 600-800 r/min; in the step (3), heating to 95-120 ℃ for reaction; the reaction time is 2-3 h.
10. The preparation method of the coated modified zinc powder as defined in any one of claims 2-9, wherein in the step (4), the calcining temperature is 300-400 ℃, and the calcining time is 2-3 h.
CN202210481592.8A 2022-05-05 2022-05-05 Coated modified zinc powder and preparation method thereof Active CN114773891B (en)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101391305A (en) * 2008-11-04 2009-03-25 昆明海创兴科技有限公司 Manufacture method of superfine laminar zinc powder and zinc pulp
CN102921425A (en) * 2012-11-08 2013-02-13 昆明理工大学 Method for preparing aluminum composite particles coated with nano oxygen carrying material

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101391305A (en) * 2008-11-04 2009-03-25 昆明海创兴科技有限公司 Manufacture method of superfine laminar zinc powder and zinc pulp
CN102921425A (en) * 2012-11-08 2013-02-13 昆明理工大学 Method for preparing aluminum composite particles coated with nano oxygen carrying material

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