CN115612323B - Preparation method of industrial protective inorganic coating - Google Patents
Preparation method of industrial protective inorganic coating Download PDFInfo
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- 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
- C09D1/00—Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances
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- C—CHEMISTRY; METALLURGY
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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
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- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
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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
- 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
Abstract
The invention discloses a preparation method of an industrial protective inorganic coating, which is characterized in that AlPO is synthesized firstly 4 As a coating base material, and then preparing a coating containing Fe 3 Fe-Al functional filler of Al intermetallic compound phase, and porous Fe is coated on the surface of MgO whisker 2 O 3 /Al 2 O 3 The composite film is used as a slow-release curing agent, the curing agent is added into the base material and the filler to be mixed to form a coating, and the coating is sprayed on the surface of the high-temperature alloy matrix and then cured at normal temperature. The invention solves the problems of uncontrollable solidification, poor high-temperature oxidation resistance and the like existing in the existing preparation of the industrial protective coating, and can be used in the field of high-temperature corrosion protection of metals.
Description
Technical Field
The invention relates to a preparation method of a coating, in particular to a preparation method of an industrial protective inorganic coating, and belongs to the field of surface engineering.
Background
In the fields of aerospace, automobiles, metallurgical engineering and constructional engineering, the service environments of various metal material parts are increasingly harsh, and the requirements on wear resistance, corrosion resistance, oxidation resistance and the like are increasingly high. In order to prolong the service life of the metal material, a coating with excellent performance is usually required to be prepared on the surface of the metal material so as to meet the use requirement of complex and severe working conditions. The organic coating has the problems of poor high temperature resistance, heat resistance, poor mechanical properties, toxicity and the like. Inorganic coatings are increasingly being used because of their high temperature resistance, corrosion resistance, non-toxicity, non-pollution and the like. In particular, phosphate coatings have the advantages of low cure shrinkage, better water resistance, etc., so that they are receiving more attention. CN110016244a discloses a high temperature resistant anti-corrosion smooth coating for stainless steel blade surface and its preparation method, the coating adopts phosphate and silica sol as film forming material, adopts modified orthophosphate or polyphosphate powder as anti-corrosion filler, selects mica powder, talcum powder, alumina powder and the like as high temperature resistant filler, strictly controls particle size distribution of filler, adds surface auxiliary agents such as wetting dispersant, surface slip agent and the like to prepare coating, then sprays on stainless steel blade surface, dries at room temperature for at least 20min; heating the dried workpiece to 70-90 ℃ and keeping the temperature for at least 15min; continuously heating to 330-350 ℃, and maintaining for at least 30min so as to prepare the smooth coating by heating and curing. CN103319919B discloses a mica and graphene co-modified inorganic coating and a use method thereof, which aims to solve the problem of poor adhesion of the existing inorganic coating on the metal surface. The invention is obtained by modifying inorganic paint with mica and graphene, wherein the added amount of the graphene accounts for 0.1-3% of the inorganic paint by mass, and the added amount of the mica accounts for 0.1-5% of the inorganic paint by mass. Directly coating the mica and graphene co-modified inorganic coating on the metal surface, and drying at room temperature to 200 ℃ for 1 minute to 24 hours; and (3) further carrying out high-temperature baking after the drying treatment, wherein the baking temperature is 200-1000 ℃ and the baking time is 1-60 minutes. At present, two major problems exist in the industrial protective inorganic phosphate coating, namely, in the preparation process of the coating, a high heating temperature is needed to realize the curing of the coating, and the coating is limited by the size and shape of a workpiece, so that the heat curing treatment after the coating is very inconvenient to construct, and the application of the coating in engineering is prevented. If the curing agent is added, the curing temperature can be reduced, even the curing is performed at normal temperature, but the curing time is too short and even the curing is completed within a few seconds, which cannot guarantee the coating construction process. The second problem is that its protective properties, in particular the resistance to high temperatures and oxidation, are inadequate, which also results in limited applications. Therefore, it is very important to develop a method for preparing an industrial protective coating with controllable curing process, low curing temperature and excellent oxidation resistance.
Disclosure of Invention
Aiming at the problems of uncontrollable solidification, poor performance and the like existing in the prior preparation of industrial protective inorganic phosphate coatingThe problem is that AlPO is synthesized firstly 4 As a coating base material, and then preparing a coating containing Fe 3 Fe-Al functional filler of Al intermetallic compound phase, and porous Fe is coated on the surface of MgO whisker 2 O 3 /Al 2 O 3 The composite film is used as a slow-release curing agent, the curing agent is added into the base material and the filler to be mixed to form a coating, and the coating is sprayed on the surface of the metal matrix and then is cured at normal temperature, so that the high-performance industrial protective inorganic coating is prepared.
The preparation method of the industrial protective inorganic coating is characterized by comprising the following steps in sequence:
（1）AlPO 4 preparing a coating base material: by H 3 PO 4 With Al (OH) 3 Preparing a coating base material by using the raw materials, weighing the raw materials according to a molar ratio of 1:1, adding the raw materials into a beaker to form a mixed solution, placing the beaker containing the mixed solution into a water bath kettle, and stirring at 90-95 ℃ for 60-90 min to react to generate AlPO 4 Cooling the phase to room temperature to obtain AlPO 4 A coating base material;
(2) Preparing Fe-Al functional filler: carbonyl Fe powder with granularity of 1-5 mu m and Al powder with granularity of 4-10 mu m are weighed according to a molar ratio of Fe to Al=2:1-1:1, and mixed in a planetary ball mill for ball milling for 30-60 min to prepare the Fe-containing powder 3 Mixed powder of Al intermetallic compound phases; adding Al powder with the thickness of 4-10 mu m into the mixed powder, controlling the addition amount of the Al powder to be 40-50% of the mass of the original mixed powder, and then mixing the mixed powder in a three-dimensional mixer for 10-30 min to obtain Fe-Al functional filler;
(3) Preparing a coating slow-release curing agent: in a first step, al (OC 3 H 7 ) 3 Adding 100ml of mixed solution with the weight percent of 5-15% into deionized water, heating and stirring the obtained mixed solution in a water bath with the temperature of 80-85 ℃ for 30-60 min to obtain a white suspension, adding 0.1-0.15 ml of concentrated nitric acid into the white suspension, heating and stirring in a water bath with the temperature of 85-95 ℃ for 5-6 h to carry out peptization reaction, and obtaining transparent Al (OH) after the peptization reaction is finished 3 Sol; second, 5-10 wt.% FeCl is prepared 3 Aqueous solution, and 5-10 ml FeCl 3 Dropping the solution into boiling 100ml deionized water under stirring, and adding dropwiseAfter the completion, boiling is continued for 3 to 5 minutes, and heating is finished to obtain Fe (OH) 3 Sol; thirdly, weighing MgO whiskers, adding the MgO whiskers into absolute ethyl alcohol to prepare 10-15 wt.% mixed solution, and performing ultrasonic dispersion treatment for 30-60 min to form MgO whisker mixed solution; fourth, according to the volume ratio of 1:1:0.5:0.5 proportion of Fe (OH) 3 Sol, al (OH) 3 Mixing sol, absolute ethyl alcohol and MgO whisker, and weighing Fe (OH) 3 Sol, al (OH) 3 Mixing the sol and absolute ethyl alcohol, stirring for 10-30 min, adding 3-5 vol% of hexadecyl trimethyl ammonium bromide, continuously stirring in a water bath at 85-95 ℃ for 1-2 h, and carrying out phase separation reaction in the mixed sol to form a phase-separated mixed sol containing two conjugated phases, namely Fe 2 O 3 /Al 2 O 3 A conjugated phase A mainly composed of an oligomer and hexadecyl trimethyl ammonium bromide, and a conjugated phase B mainly composed of a solvent mixture; fifthly, adding the phase-separated mixed sol into the measured MgO whisker mixed solution, and continuously stirring for 1-2 hours in a water bath at 85-95 ℃ to enable the phase-separated mixed sol to be coated on the surface of the MgO whisker; sixthly, placing MgO whisker coated with the mixed sol on the surface into a muffle furnace for heat treatment, preserving heat at 100-110 ℃ for 1-2 h to remove conjugate phase B, preserving heat at 450-550 ℃ for 2h to remove hexadecyl trimethyl ammonium bromide in the conjugate phase A, and converting the mixed sol on the surface of MgO whisker into Fe with a porous structure 2 O 3 /Al 2 O 3 Grinding the heat-treated product into powder, sieving the powder by 400 meshes to obtain the coating slow-release curing agent with the specific surface of 45-60 m 2 The pore diameter of the curing agent composite layer is 50-400 nm;
(4) Air spraying and room temperature curing of the coating: firstly, preprocessing a coating matrix, carrying out sand blasting treatment on high-temperature alloy GH4169 for 2-5 min, carrying out ultrasonic cleaning in absolute ethyl alcohol for 10-20 min, and drying at 85-95 ℃ for 30-40 min; then preparing a coating, and adding AlPO 4 The coating base material, the slow-release curing agent and the Fe-Al functional filler are mixed according to the mass ratio of 10: (0.5 to 1.5): (0.1-0.5), and stirring for 5-15 min at room temperature to form a coating; after the paint is prepared, the air spraying mode is adopted to prepare the coating on the surface of the high-temperature alloy matrix in 10 h, and the spraying gas is adoptedThe pressure is controlled to be 0.45-0.55 MPa, the spraying amount of the coating is controlled to be 180-200 ml/min, the spraying distance is 200-250 mm, the gun conveying speed is 300-400 mm/s, the spraying width is 100-150 mm, the overlapping rate of the spraying width in the adjacent stroke is 30% -50%, the sprayed coating is placed at room temperature for 36-60 h, the coating curing is completed, and the weight loss rate of 24h after the curing is completed is less than or equal to 0.05%.
The preparation method of the industrial protective inorganic coating is further characterized in that:
(1) Preparation of AlPO 4 When the base material is coated, the stirring speed is 100-200 r/min;
(2) When the Fe-Al functional filler is prepared, the rotating speed of planetary ball milling is 300-350 r/min, a stainless steel ball with the diameter of 5mm is adopted, and the mass ratio of the ball materials is (3-5): 1, firstly vacuumizing the ball pot to be lower than 1 multiplied by 10 during ball milling -2 Pa, and then filling high-purity Ar gas of 0.10-0.12 MPa for protection; the rotating speed of the three-dimensional mixer is 10-20 r/min;
(3) The stirring speed is 100-200 r/min in the process of preparing the coating slow-release curing agent; mgO whisker has a length of 600-800 mu m and a diameter of 5-10 mu m, and the ultrasonic frequency and power of MgO whisker during ultrasonic dispersion treatment are 40 kHz and 100W respectively; the temperature rising rate of MgO whisker coated with mixed sol on the surface is 5-10 ℃/min when the MgO whisker is subjected to heat treatment in a muffle furnace;
(4) When the high-temperature alloy GH4169 is subjected to sand blasting treatment, the granularity of brown corundum adopted is 46-80 meshes, the air inlet pressure is 0.5-0.7 MPa, and the sand blasting distance is 80-100 mm; the ultrasonic frequency and power of the matrix during ultrasonic cleaning treatment are respectively 40 kHz and 100W; the stirring speed is 100-200 r/min when the coating is prepared.
The invention has the advantages that: (1) The invention provides a method for coating porous Fe on the surface of MgO whisker 2 O 3 /Al 2 O 3 The composite layer is used as a curing agent, and the porous structure plays a role of slow release so as to realize the controllable curing process of the coating, thereby avoiding rapid curing. (2) In the coating prepared by the method, the coating base material AlPO 4 A phase containing Fe 3 The functional filler of the Al intermetallic compound can improve the high-temperature oxidation resistance of the coating and can form Al in a high-temperature working condition 2 O 3 The film plays a good protective role. (3) MgO whisker surface coatingFe 2 O 3 /Al 2 O 3 Layer and Fe/Al filler and Al formed by pre-oxidation 2 O 3 And the physical properties and chemical properties of the coating are similar, and the matching of the thermal expansion coefficient and the proper matching of chemical bonds can avoid the formation of cracks in the coating. (4) After MgO whisker is added, a cross network can be formed in the coating, which is beneficial to obtaining high coating strength, hardness and tissue uniformity.
Drawings
FIG. 1 is a schematic diagram of a process for preparing an industrial protective inorganic coating according to the present invention.
Detailed Description
Example 1: the industrial protective inorganic coating is prepared according to the following steps
（1）AlPO 4 Preparing a coating base material: by H 3 PO 4 With Al (OH) 3 Preparing a coating base material by using the raw materials, weighing the raw materials according to a molar ratio of 1:1, adding the raw materials into a beaker to form a mixed solution, placing the beaker containing the mixed solution into a water bath kettle, and stirring for 65 min at 90 ℃ to react to generate AlPO 4 The phase, stirring rate is 120 r/min, and cooling to room temperature to obtain AlPO 4 A coating base material;
(2) Preparing Fe-Al functional filler: carbonyl Fe powder with the granularity of 2 mu m and Al powder with the granularity of 5 mu m are weighed according to the mol ratio Fe:Al=2:1 and mixed in a planetary ball mill, the rotating speed of the planetary ball mill is 300 r/min, a stainless steel ball with the diameter of 5mm is adopted, and the mass ratio of the ball materials is 4:1, firstly vacuumizing the ball pot to be lower than 1 multiplied by 10 during ball milling -2 Pa, filling high-purity Ar gas of 0.10 MPa for protection, and ball milling for 35min to prepare the Fe-containing alloy 3 Mixed powder of Al intermetallic compound phases; adding 5 mu m Al powder into the mixed powder, controlling the adding amount of the Al powder to be 40% of the mass of the original mixed powder, and then mixing the mixed powder in a three-dimensional mixer for 15min, wherein the rotating speed of the three-dimensional mixer is 12 r/min, so as to obtain Fe-Al functional filler;
(3) Preparing a coating slow-release curing agent: in a first step, al (OC 3 H 7 ) 3 Adding into deionized water to form 7. 7 wt.% mixed solution 100ml, heating the obtained mixed solution in 80deg.C water bath, stirring for 35min at stirring rate of 120 r/min to obtain white suspension, and making into desired dosage formAdding 0.1ml of concentrated nitric acid into the color suspension, heating in water bath at 85deg.C and stirring for 5 hr for peptization reaction at stirring rate of 150r/min to obtain transparent Al (OH) after peptization reaction 3 Sol; in the second step, 6wt.% FeCl is prepared 3 Aqueous solution, and 6ml FeCl 3 Dropping the solution into 100ml of boiled deionized water, and continuously stirring at a stirring rate of 130 r/min, and continuously boiling for 3min to finish heating to obtain Fe (OH) 3 Sol; thirdly, weighing MgO whisker, adding the MgO whisker into absolute ethyl alcohol to prepare a mixed solution with the weight percentage of 12%, carrying out ultrasonic dispersion treatment on MgO whisker with the length of 600-800 mu m and the diameter of 5-10 mu m, wherein the ultrasonic frequency and power during ultrasonic dispersion treatment are respectively 40 kHz and 100W, and forming MgO whisker mixed solution after ultrasonic treatment for 35min; fourth, according to the volume ratio of 1:1:0.5:0.5 proportion of Fe (OH) 3 Sol, al (OH) 3 Mixing sol, absolute ethyl alcohol and MgO whisker, and weighing Fe (OH) 3 Sol, al (OH) 3 Mixing and stirring the sol and absolute ethyl alcohol at a stirring speed of 140r/min, adding 3vol% of hexadecyl trimethyl ammonium bromide after stirring for 12min, continuously stirring for 1h in a water bath at 85 ℃, and carrying out phase separation reaction in the mixed sol at a stirring speed of 160r/min to form a phase separation mixed sol containing two conjugated phases, namely Fe 2 O 3 /Al 2 O 3 A conjugated phase A mainly composed of an oligomer and hexadecyl trimethyl ammonium bromide, and a conjugated phase B mainly composed of a solvent mixture; fifthly, adding the phase-separated mixed sol into the measured MgO whisker mixed solution, and continuously stirring for 1h in a water bath at 85 ℃ to enable the phase-separated mixed sol to be coated on the surface of MgO whisker, wherein the stirring speed is 160r/min; sixthly, placing MgO whisker coated with the mixed sol on the surface into a muffle furnace for heat treatment, wherein the heating rate is 5 ℃/min, maintaining the temperature at 100 ℃ for 1h to remove the conjugated phase B, maintaining the temperature at 450 ℃ for 2h to remove hexadecyl trimethyl ammonium bromide in the conjugated phase A, and converting the mixed sol on the surface of the MgO whisker into Fe with a porous structure 2 O 3 /Al 2 O 3 Grinding the heat-treated product into powder, sieving with 400 mesh sieve to obtain the final product with a specific surface of 51m 2 The pore diameter of the curing agent composite layer is 50-350 nm;
(4) Air spraying and room temperature curing of the coating: firstly, preprocessing a coating matrix, carrying out sand blasting on high-temperature alloy GH4169 for 3min, adopting brown corundum with granularity of 46 meshes, air inlet pressure of 0.5 MPa and sand blasting distance of 80. 80mm, carrying out ultrasonic cleaning in absolute ethyl alcohol for 10 min after sand blasting, respectively carrying out ultrasonic frequency and power on the matrix during ultrasonic cleaning treatment at 40 kHz and 100W, and then drying at 85 ℃ for 30min; then preparing a coating, and adding AlPO 4 The coating base material, the slow-release curing agent and the Fe-Al functional filler are mixed according to the mass ratio of 10:0.5: mixing and stirring at room temperature at a stirring rate of 130 r/min for 6min to form a coating; the method comprises the steps of preparing a coating on the surface of a high-temperature alloy matrix in 5 hours after the preparation of the coating by adopting an air spraying mode, controlling the spraying air pressure to be 0.45MPa, controlling the spraying amount of the coating to be 180ml/min, controlling the spraying distance to be 210 mm, controlling the gun conveying speed to be 310 mm/s, controlling the spraying width to be 100 mm, controlling the overlap ratio of the spraying width in the adjacent stroke to be 35%, setting the sprayed coating at room temperature to be 50 h, completing the solidification of the coating, and controlling the weight loss ratio to be less than or equal to 0.05% after the solidification is completed in 24 hours.
Example 2: the industrial protective inorganic coating is prepared according to the following steps
（1）AlPO 4 Preparing a coating base material: by H 3 PO 4 With Al (OH) 3 Preparing a coating base material by using the raw materials, weighing the raw materials according to a molar ratio of 1:1, adding the raw materials into a beaker to form a mixed solution, placing the beaker containing the mixed solution into a water bath kettle, and stirring for 85 min at 95 ℃ to react to generate AlPO 4 The phase, stirring rate is 180 r/min, and cooling to room temperature to obtain AlPO 4 A coating base material;
(2) Preparing Fe-Al functional filler: carbonyl Fe powder with the granularity of 5 mu m and Al powder with the granularity of 8 mu m are weighed according to the mol ratio Fe:Al=1:1 and mixed in a planetary ball mill, the rotating speed of the planetary ball mill is 350 r/min, a stainless steel ball with the diameter of 5mm is adopted, and the mass ratio of the ball materials is 5:1, firstly vacuumizing the ball pot to be lower than 1 multiplied by 10 during ball milling -2 Pa, filling high-purity Ar gas of 0.12 MPa for protection, and ball milling for 60min to prepare the Fe-containing alloy 3 Mixed powder of Al intermetallic compound phases; adding 8 μm Al powder into the mixed powder, controlling the addition amount of Al powder to be 50% of the mass of the original mixed powder, and thenMixing for 30min in a three-dimensional mixer, wherein the rotating speed of the three-dimensional mixer is 18r/min, and obtaining Fe-Al functional filler;
(3) Preparing a coating slow-release curing agent: in a first step, al (OC 3 H 7 ) 3 Adding into deionized water to form 13wt.% mixed solution 100ml, heating and stirring the obtained mixed solution in water bath at 85deg.C for 55min at stirring rate of 170 r/min to obtain white suspension, adding 0.14ml concentrated nitric acid into the white suspension, heating and stirring in water bath at 90deg.C for 6 h to perform peptization reaction at stirring rate of 190 r/min to obtain transparent Al (OH) after peptization reaction 3 Sol; in the second step, 8wt.% FeCl is prepared 3 Aqueous solution, and 9 ml FeCl 3 Dropping the solution into 100ml of boiled deionized water and continuously stirring at a stirring rate of 200 r/min, and continuously boiling for 5min after the dropping is completed to finish heating to obtain Fe (OH) 3 Sol; thirdly, weighing MgO whisker, adding the MgO whisker into absolute ethyl alcohol to prepare a mixed solution with the weight of 14%, carrying out ultrasonic dispersion treatment on MgO whisker with the length of 600-800 mu m and the diameter of 5-10 mu m, wherein the ultrasonic frequency and power during ultrasonic dispersion treatment are respectively 40 kHz and 100W, and forming MgO whisker mixed solution after ultrasonic treatment for 50 min; fourth, according to the volume ratio of 1:1:0.5:0.5 proportion of Fe (OH) 3 Sol, al (OH) 3 Mixing sol, absolute ethyl alcohol and MgO whisker, and weighing Fe (OH) 3 Sol, al (OH) 3 Mixing and stirring the sol and absolute ethyl alcohol at a stirring speed of 180 r/min, adding 5vol% of hexadecyl trimethyl ammonium bromide after stirring for 25min, continuously stirring for 1.5h in a water bath at 90 ℃ at a stirring speed of 160r/min, and carrying out phase separation reaction in the mixed sol to form a phase separation mixed sol containing two conjugate phases, namely Fe 2 O 3 /Al 2 O 3 A conjugated phase A mainly composed of an oligomer and hexadecyl trimethyl ammonium bromide, and a conjugated phase B mainly composed of a solvent mixture; fifthly, adding the phase-separated mixed sol into the measured MgO whisker mixed solution, and continuously stirring for 2 hours in a water bath at 92 ℃ to enable the phase-separated mixed sol to be coated on the surface of MgO whisker, wherein the stirring speed is 160r/min; sixthly, putting MgO whisker coated with the mixed sol into a muffle furnace for heat treatment, and heatingAt a speed of 8 ℃/min, preserving heat for 2 hours at 105 ℃ to remove the conjugated phase B, preserving heat for 2 hours at 500 ℃ to remove hexadecyl trimethyl ammonium bromide in the conjugated phase A, so that the mixed sol on the surface of the MgO whisker is converted into Fe with a porous structure 2 O 3 /Al 2 O 3 Grinding the heat-treated product into powder, sieving with 400 mesh sieve to obtain the coating slow-release curing agent with a specific surface of 56m 2 The pore diameter of the curing agent composite layer is 50-380 nm;
(4) Air spraying and room temperature curing of the coating: firstly, preprocessing a coating matrix, carrying out sand blasting on high-temperature alloy GH4169 for 4 min, adopting brown corundum with granularity of 80 meshes, air inlet pressure of 0.7 MPa and sand blasting distance of 100 mm, carrying out ultrasonic cleaning in absolute ethyl alcohol for 20min after sand blasting, respectively carrying out ultrasonic frequency and power on the matrix during ultrasonic cleaning treatment at 40 kHz and 100W, and then drying at 90 ℃ for 35min; then preparing a coating, and adding AlPO 4 The coating base material, the slow-release curing agent and the Fe-Al functional filler are mixed according to the mass ratio of 10:1.5:0.3 mixing and stirring at room temperature at a stirring rate of 200 r/min for 14 min to form a coating; after the paint is prepared, the air spraying mode is adopted to prepare the coating on the surface of the high-temperature alloy matrix within 2 hours, the spraying air pressure is controlled at 0.50 MPa, the paint spraying amount is controlled at 200 ml/min, the spraying distance is 230 mm, the gun conveying speed is 380mm/s, the spraying width is 150 mm, the overlapping rate of the spraying width in the adjacent stroke is 40%, the sprayed coating is placed at room temperature for 40 hours to finish the curing of the coating, and the weight loss rate of 24 hours after the curing is finished is less than or equal to 0.05%.
Claims (2)
1. The preparation method of the industrial protective inorganic coating is characterized by comprising the following steps in sequence:
（1）AlPO 4 preparing a coating base material: by H 3 PO 4 With Al (OH) 3 Preparing a coating base material by using the raw materials, weighing the raw materials according to a molar ratio of 1:1, adding the raw materials into a beaker to form a mixed solution, placing the beaker containing the mixed solution into a water bath kettle, and stirring at 90-95 ℃ for 60-90 min to react to generate AlPO 4 Cooling the phase to room temperature to obtain AlPO 4 A coating base material;
(2) Preparing Fe-Al functional filler: massaging deviceThe carbonyl Fe powder with the granularity of 1-5 mu m and the Al powder with the granularity of 4-10 mu m are weighed according to the molar ratio Fe:Al=2:1-1:1, and are mixed in a planetary ball mill for ball milling for 30-60 min to prepare the Fe-containing powder 3 Mixed powder of Al intermetallic compound phases; adding Al powder with the thickness of 4-10 mu m into the mixed powder, controlling the addition amount of the Al powder to be 40-50% of the mass of the original mixed powder, and then mixing the mixed powder in a three-dimensional mixer for 10-30 min to obtain Fe-Al functional filler;
(3) Preparing a coating slow-release curing agent: in a first step, al (OC 3 H 7 ) 3 Adding 100mL of mixed solution with the weight percent of 5-15% into deionized water, heating and stirring the obtained mixed solution in a water bath with the temperature of 80-85 ℃ for 30-60 min to obtain a white suspension, adding 0.1-0.15 mL of concentrated nitric acid into the white suspension, heating and stirring in a water bath with the temperature of 85-95 ℃ for 5-6 h to carry out peptization reaction, and obtaining transparent Al (OH) after the peptization reaction is finished 3 Sol; secondly, preparing 5-10wt% of FeCl 3 Aqueous solution, and 5-10 mL FeCl 3 Dropwise adding the solution into 100mL of boiled deionized water, continuously stirring, and continuously boiling for 3-5 min after the dropwise adding is finished to finish heating to obtain Fe (OH) 3 Sol; thirdly, weighing MgO whiskers, adding the MgO whiskers into absolute ethyl alcohol to prepare 10-15wt% mixed solution, and performing ultrasonic dispersion treatment for 30-60 min to form MgO whisker mixed solution; fourth, according to the volume ratio of 1:1:0.5:0.5 proportion of Fe (OH) 3 Sol, al (OH) 3 Mixing sol, absolute ethyl alcohol and MgO whisker, and weighing Fe (OH) 3 Sol, al (OH) 3 Mixing the sol and absolute ethyl alcohol, stirring for 10-30 min, adding 3-5 vol% of hexadecyl trimethyl ammonium bromide, continuously stirring in a water bath at 85-95 ℃ for 1-2 h, and carrying out phase separation reaction in the mixed sol to form a phase-separated mixed sol containing two conjugate phases, namely Fe 2 O 3 /Al 2 O 3 A conjugated phase A mainly composed of an oligomer and hexadecyl trimethyl ammonium bromide, and a conjugated phase B mainly composed of a solvent mixture; fifthly, adding the phase-separated mixed sol into the measured MgO whisker mixed solution, and continuously stirring for 1-2 hours in a water bath at 85-95 ℃ to enable the phase-separated mixed sol to be coated on the surface of the MgO whisker; sixth, mgO whisker coated with mixed sol is put into a muffle furnaceHeat treatment is carried out, the temperature is kept at 100-110 ℃ for 1-2 h to remove the conjugated phase B, and the temperature is kept at 450-550 ℃ for 2h to remove cetyl trimethyl ammonium bromide in the conjugated phase A, so that mixed sol on the surface of MgO whisker is converted into Fe with a porous structure 2 O 3 /Al 2 O 3 Grinding the heat-treated product into powder, sieving the powder by 400 meshes to obtain the coating slow-release curing agent with the specific surface of 45-60 m 2 The pore diameter of the curing agent composite layer is 50-400 nm;
(4) Air spraying and room temperature curing of the coating: firstly, preprocessing a coating matrix, carrying out sand blasting treatment on high-temperature alloy GH4169 for 2-5 min, carrying out ultrasonic cleaning in absolute ethyl alcohol for 10-20 min, and drying at 85-95 ℃ for 30-40 min; then preparing a coating, and adding AlPO 4 The coating base material, the slow-release curing agent and the Fe-Al functional filler are mixed according to the mass ratio of 10: (0.5 to 1.5): (0.1-0.5), and stirring for 5-15 min at room temperature to form a coating; after the paint is prepared, the air spraying mode is adopted to prepare the coating on the surface of the high-temperature alloy matrix in a 10 h mode, the spraying air pressure is controlled to be 0.45-0.55 MPa, the paint spraying amount is controlled to be 180-200 mL/min, the spraying distance is 200-250 mm, the gun conveying speed is 300-400 mm/s, the spraying width is 100-150 mm, the overlapping rate of the spraying width in the adjacent stroke is 30-50%, the sprayed coating is placed at room temperature for 36-60 h to finish the curing of the coating, and the weight loss rate of 24h after the curing is finished is less than or equal to 0.05%.
2. The method of preparing an industrial protective inorganic coating according to claim 1, further characterized by:
(1) Preparation of AlPO 4 When the base material is coated, the stirring speed is 100-200 r/min;
(2) When the Fe-Al functional filler is prepared, the rotating speed of planetary ball milling is 300-350 r/min, a stainless steel ball with the diameter of 5mm is adopted, and the mass ratio of the ball materials is (3-5): 1, firstly vacuumizing the ball pot to be lower than 1 multiplied by 10 during ball milling -2 Pa, and then filling high-purity Ar gas of 0.10-0.12 MPa for protection; the rotating speed of the three-dimensional mixer is 10-20 r/min;
(3) The stirring speed is 100-200 r/min in the process of preparing the coating slow-release curing agent; mgO whisker has a length of 600-800 mu m and a diameter of 5-10 mu m, and the ultrasonic frequency and power of MgO whisker during ultrasonic dispersion treatment are 40 kHz and 100W respectively; the temperature rising rate of MgO whisker coated with mixed sol on the surface is 5-10 ℃/min when the MgO whisker is subjected to heat treatment in a muffle furnace;
(4) When the high-temperature alloy GH4169 is subjected to sand blasting treatment, the granularity of brown corundum adopted is 46-80 meshes, the air inlet pressure is 0.5-0.7 MPa, and the sand blasting distance is 80-100 mm; the ultrasonic frequency and power of the matrix during ultrasonic cleaning treatment are respectively 40 kHz and 100W; the stirring speed is 100-200 r/min when the coating is prepared.
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| JPS6438482A (en) * | 1987-08-03 | 1989-02-08 | Teikoku Kako Co Ltd | Rust-preventive coating composition |
| CN101531833A (en) * | 2009-04-21 | 2009-09-16 | 无锡菲科尔生态环保科技有限公司 | Non-toxic infrared reflecting paint and preparation method thereof |
| CN102443796A (en) * | 2011-12-02 | 2012-05-09 | 九江学院 | Porous Fe-Al intermetallic compound coating and its preparation method |
| CN110776761A (en) * | 2019-10-31 | 2020-02-11 | 烟台龙源电力技术股份有限公司 | Composite gradient coating and ceramic paint product |
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| US20090075083A1 (en) * | 1997-07-21 | 2009-03-19 | Nanogram Corporation | Nanoparticle production and corresponding structures |
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|---|---|---|---|---|
| JPS6438482A (en) * | 1987-08-03 | 1989-02-08 | Teikoku Kako Co Ltd | Rust-preventive coating composition |
| CN101531833A (en) * | 2009-04-21 | 2009-09-16 | 无锡菲科尔生态环保科技有限公司 | Non-toxic infrared reflecting paint and preparation method thereof |
| CN102443796A (en) * | 2011-12-02 | 2012-05-09 | 九江学院 | Porous Fe-Al intermetallic compound coating and its preparation method |
| CN110776761A (en) * | 2019-10-31 | 2020-02-11 | 烟台龙源电力技术股份有限公司 | Composite gradient coating and ceramic paint product |
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