CN108587423B - Magnesium alloy ingot surface cleaning method - Google Patents
Magnesium alloy ingot surface cleaning method Download PDFInfo
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- CN108587423B CN108587423B CN201810449093.4A CN201810449093A CN108587423B CN 108587423 B CN108587423 B CN 108587423B CN 201810449093 A CN201810449093 A CN 201810449093A CN 108587423 B CN108587423 B CN 108587423B
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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
- C09D167/00—Coating compositions based on polyesters obtained by reactions forming a carboxylic ester link in the main chain; Coating compositions based on derivatives of such polymers
- C09D167/08—Polyesters modified with higher fatty oils or their acids, or with natural resins or resin acids
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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
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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
- C09D7/70—Additives characterised by shape, e.g. fibres, flakes or microspheres
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/16—Halogen-containing compounds
- C08K2003/166—Magnesium halide, e.g. magnesium chloride
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2296—Oxides; Hydroxides of metals of zinc
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/003—Additives being defined by their diameter
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/004—Additives being defined by their length
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- Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)
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Abstract
The invention discloses a magnesium alloy ingot surface cleaning method, which comprises the following steps: step one, preparing a component A containing alkyd resin, wherein the alkyd resin is self-made; step two, uniformly mixing the component A and an alkyd resin curing agent to prepare a cleaning solution, immediately soaking a cast mother alloy ingot obtained after casting in the cleaning solution, and taking out the ingot after a coating layer is formed on the surface of the ingot; the addition amount of the alkyd resin curing agent is 8-15% of the mass of the alkyd resin in the first step; and step three, drying the surface of the cast ingot at the temperature of 80-100 ℃, and tearing off the solidified coating layer by using external force when the temperature is reduced to 30-40 ℃ after drying to obtain the master alloy cast ingot with the surface cleaned. According to the cleaning method, the coating layer with certain adsorption performance and oil removal performance is formed on the surface of the magnesium alloy ingot to be treated by utilizing the matching of special materials and the solidification characteristic of a high polymer material, and then the coating layer is torn off by utilizing the characteristic of easy separation between the coating layer and the magnesium alloy ingot body, so that the dirt on the surface of the magnesium alloy ingot is also removed while the coating layer is torn off.
Description
Technical Field
The invention belongs to the technical field of magnesium alloy, and particularly relates to a magnesium alloy ingot surface cleaning method.
Background
The magnesium alloy is formed by adding other elements based on magnesium element, and is characterized in that: the aluminum alloy has the advantages of small density, high strength, large elastic modulus, good heat dissipation performance, good shock absorption, larger impact load bearing capacity than aluminum alloy, and good organic matter and alkali corrosion resistance. The main alloy elements include aluminum, zinc, manganese, cerium, thorium and a small amount of zirconium or cadmium. At present, the most widely used is magnesium-aluminum alloy, and then magnesium-manganese alloy and magnesium-zinc-zirconium alloy, which are mainly applied to aviation, aerospace, transportation, chemical engineering, rocket and other industrial departments. The cast magnesium alloy is formed by adding alloying elements into magnesium as a base, and is suitable for producing parts by a casting method. According to the forming process, magnesium alloys can be divided into cast magnesium alloys and wrought magnesium alloys, which have great differences in composition and structure properties. The cast magnesium alloy is mainly used for automobile parts, machine part shells, electric components and the like.
The surface of the magnesium alloy ingot is easily polluted in the manufacturing process, such as oil (mechanical oil, lubricating oil, die oil and the like) and processing raw material scraps, and meanwhile, if the temperature is not reduced in time in the processing and producing process, oxides are easily generated on the surface of the ingot. In the prior art, a cleaning agent is often adopted to clean the surface of the magnesium alloy ingot, such as by using organic matters. The organic cleaning agent can quickly remove oil stains, but easily causes carbon residue on the surface of a magnesium alloy ingot, influences the carbon content in a workpiece in the subsequent casting process of utilizing the ingot, and has great trouble on the stability of chemical components of a cast magnesium alloy workpiece. And certain loss can be caused to the aluminum alloy body by using an acid washing or alkali washing mode, and particularly, the surface form of the magnesium alloy is easy to damage by using an alkali washing process, so that secondary corrosion is caused.
Disclosure of Invention
In order to solve the defects of the prior art, the invention provides a surface cleaning method for a magnesium alloy ingot, which comprises the steps of forming a wrapping layer with certain adsorption performance and oil removal performance on the surface of the magnesium alloy ingot to be treated by utilizing the matching of special materials and the solidification characteristic of a medium-high molecular material, tearing off the wrapping layer by utilizing the characteristic of easy separation between the wrapping layer and a magnesium alloy ingot body, removing the dirt on the surface of the magnesium alloy ingot while tearing off the wrapping layer, and simultaneously not generating any influence on the surface of the magnesium alloy ingot.
The technical effect to be achieved by the invention is realized by the following scheme:
the magnesium alloy ingot surface cleaning method provided by the invention comprises the following steps:
step one, weighing raw materials according to the following components in parts by weight to prepare a component A:
4-6 parts of magnesium chloride
3-6 parts of high silica glass fiber
6-8 parts of zinc oxide
28-30 parts of alkyd resin
2-3 parts of magnesium silicate hydroxide
2-3 parts of sodium bisulfate
1-2 parts of aluminum potassium sulfate
3-4 parts of expanded graphite powder
0.02-0.03 part of paraffin with 25-30 carbon atoms
The preparation method of the alkyd resin comprises the following steps: mixing rice bran oil and n-butanol, heating to 115-120 ℃, dropwise adding a saturated lithium hydroxide solution as a catalyst, and continuously heating to 250 ℃ for reaction for 4-6 h; cooling to 120 ℃ after the reaction is finished, then adding phthalic anhydride and ethanol, heating to 160 ℃ for reaction for 4-6h after the reaction is finished, cooling to 50-60 ℃ after the reaction is finished, then dropwise adding mixed TDI and xylene, heating to 105 ℃ after the dropwise adding is finished, reacting for 6-8h, cooling to 50-60 ℃ after the reaction is finished, then adding ethylene glycol, keeping the temperature and stirring for 2-4h, then naturally cooling, and filtering to obtain the needed alkyd resin;
mixing the raw materials, grinding the mixture in a planetary grinder until the mixture is uniform and the size of the solid is less than 1 mu m to obtain a component A;
step two, uniformly mixing the component A and an alkyd resin curing agent to prepare a cleaning solution, immediately soaking a cast mother alloy ingot obtained after casting in the cleaning solution, and taking out the ingot after a coating layer is formed on the surface of the ingot;
the addition amount of the alkyd resin curing agent is 8-15% of the mass of the alkyd resin in the first step;
and step three, drying the surface of the cast ingot at the temperature of 80-100 ℃, and tearing off the solidified coating layer by using external force when the temperature is reduced to 30-40 ℃ after drying to obtain the master alloy cast ingot with the surface cleaned.
According to the invention, the alkyd resin and magnesium chloride are mixed to form the main body structure of the wrapping layer, so that the alkyd resin has the characteristics of good heat resistance and water resistance, good corrosion resistance and organic matter dissolution resistance, and low normal temperature strength, and is very suitable for the characteristics of needing rapid curing to improve efficiency and being easy to peel from the surface of an ingot. However, the existing alkyd resin applied to the invention still has the problem of low curing speed, so the self-made alkyd resin is adopted in the invention, the curing speed of the alkyd resin is high, the normal-temperature strength is low, and the alkyd resin is very suitable for the characteristics of needing rapid curing to improve the efficiency and being easy to strip from the surface of an ingot. The addition of the magnesium chloride can keep the electric balance between the coating layer and the magnesium alloy ingot, thereby ensuring that no adverse effect is generated on the surface of the ingot. The present inventors have found in practice that the problem of the long time required for peeling of the coating layer formed only by using the components of the resin and the curing agent is solved by the present invention, which is that the coating layer is first increased in thickness and surface friction by adding high silica glass fibers to make it easier to peel and the operation in the third step is easier.
In addition, zinc oxide powder and magnesium silicate hydroxide are added as components with a certain lubricating function, so that the prepared wrapping layer can be removed by using a proper external force under a certain temperature condition. The problem of compatibility between the solid in the component A and the alkyd resin is accompanied by the addition of the easily stripped component, if a fiber material and lubricating powder are added, the resin is easy to be layered in solid powder, and the application cannot be carried out at all, aiming at the problem, a small amount of paraffin with 25-30 carbon atoms is added as an active agent at the same time, the compatibility between the solid component and the resin is adjusted, the paraffin with 25-30 carbon atoms is environment-friendly, high-temperature resistant and very strong in permeability, and the raw material liquid with uniform components can be obtained by adding the paraffin with 25-30 carbon atoms and grinding by using a planetary grinding machine. The expanded graphite powder is a worm-like substance with a loose porous structure, has corrosion resistance and self-lubricating property, can expand greatly when meeting high temperature, improves the surface energy, greatly improves the adsorption capacity and the shaping capacity, and has very beneficial effect on removing the wrapping layer in the subsequent step. The sodium bisulfate and the aluminum potassium sulfate are acid salts, which can not generate any corrosion to the surface of the aluminum alloy cast ingot, and the use of alkaline salts is required to be avoided.
Further, in the step one, the particle sizes of the magnesium chloride, the zinc oxide, the magnesium silicate hydroxide, the sodium bisulfate, the potassium aluminum sulfate and the expanded graphite powder are 0.05 to 0.1 mu m.
Further, in the step one, the length of the high silica glass fiber is 0.5-2mm, and the diameter is 15-20 μm. The fiber should not be too long, otherwise the formation of the wrapping layer is not utilized, the diameter of the fiber also needs to be within a reasonable range, the influence on the thickness of the wrapping layer is too large if the diameter is too large, and the effect cannot be achieved if the diameter is too small.
Further, in the first step, the mass ratio of the rice bran oil, the n-butanol, the phthalic anhydride, the ethanol, the TDI, the xylene and the ethylene glycol in the alkyd resin preparation process is 1: (0.4-0.5): (0.2-0.3): (2-3): (0.2-0.25): (0.1-0.2): (0.08-0.15); the amount of saturated lithium hydroxide solution added was 1 drop per 5ml of reaction mass.
Further, in the second step, the addition amount of the alkyd resin curing agent is 10-12% of the mass of the alkyd resin in the first step.
Further, in the second step, the thickness of the wrapping layer is 300-.
Further, in the third step, the drying time is 10-15 minutes.
Further, in the third step, the temperature is reduced to 3-4 ℃/s after drying.
Further, in the third step, the hardness of the dried coating layer is in the range of 2B-2H in terms of pencil hardness. Preferably, in the third step, the hardness of the dried coating layer is HB, F or H in pencil hardness.
The invention has the following advantages:
the invention provides a surface cleaning method for a magnesium alloy ingot, which comprises the steps of forming a wrapping layer with certain adsorption performance and oil removal performance on the surface of the magnesium alloy ingot to be treated by utilizing the matching of special materials and the solidification characteristic of a high molecular material in the wrapping layer, tearing off the wrapping layer by utilizing the characteristic of easy separation between the wrapping layer and a magnesium alloy ingot body, removing the dirt on the surface of the magnesium alloy ingot while tearing off the wrapping layer, and simultaneously not generating any influence on the surface of the magnesium alloy ingot.
Detailed Description
The present invention will be described in detail with reference to examples.
In this example, the cast magnesium alloys ZM-5, ZM-7, ZM-3 and ZM-10 were chemically prepared into rod-like master alloy ingots having a uniform length of 5cm and a diameter of 1 cm. Each grade of cast magnesium alloy was prepared as a master alloy rod ingot for subsequent testing.
Example 1
The method for cleaning the surface of the magnesium alloy ingot in the embodiment comprises the following steps:
step one, weighing raw materials according to the following components in parts by weight to prepare a component A:
4 portions of magnesium chloride
6 parts of high silica glass fiber
8 portions of zinc oxide
Alkyd resin 30 parts
Magnesium hydroxy silicate 2 parts
Sodium bisulfate 2 parts
2 portions of aluminum potassium sulfate
4 portions of expanded graphite powder
0.02 portion of paraffin with 25 to 30 carbon atoms
The preparation method of the alkyd resin comprises the following steps: mixing rice bran oil and n-butanol, heating to 118 ℃, dropwise adding a saturated lithium hydroxide solution as a catalyst, and continuously heating to 250 ℃ for reaction for 4 hours; and after the reaction is finished, cooling to 118 ℃, then adding phthalic anhydride and ethanol, heating to 150 ℃, reacting for 4h, cooling to 50 ℃ after the reaction is finished, then dropwise adding mixed TDI and xylene, heating to 100 ℃ after the dropwise adding is finished, reacting for 6h, cooling to 55 ℃ after the reaction is finished, then adding glycol, keeping the temperature, stirring for 2h, naturally cooling, and filtering to obtain the needed alkyd resin. In the alkyd resin preparation process, the mass ratio of rice bran oil, n-butanol, phthalic anhydride, ethanol, TDI, xylene and ethylene glycol is 1: 0.47: 0.24: 2.05: 0.23: 0.18: 0.11; the amount of saturated lithium hydroxide solution added was 1 drop per 5ml of reaction mass.
The high silica glass fiber had a length of 1mm and a diameter of 20 μm. The particle size of the magnesium chloride, the zinc oxide, the magnesium hydroxy silicate, the sodium bisulfate, the aluminum potassium sulfate and the expanded graphite powder is 0.05 mu m.
The raw materials are mixed and ground in a planetary grinder until the mixture is uniform and the size of the solid is less than 1 mu m, thus obtaining the component A.
And step two, uniformly mixing the component A and an alkyd resin curing agent to prepare a cleaning solution, immediately soaking the cast mother alloy ingot in the cleaning solution, and taking out the ingot after a coating layer is formed on the surface of the ingot. The thickness of the coating layer was 400. mu.m. In this example, a commercially available alkyd resin curing agent (manufacturer: Basff) was used.
The addition amount of the alkyd resin curing agent is 11% of the mass of the alkyd resin in the step one.
And step three, drying the surface of the cast ingot at 90 ℃ for 15 minutes, tearing the solidified coating layer by using external force when the temperature is reduced to 40 ℃ after drying, wherein the hardness of the dried coating layer is calculated as F according to the pencil hardness, and obtaining the master alloy cast ingot with the surface cleaned, wherein the temperature of reduction after drying is 4 ℃/s.
Example 2
The cleaning procedure in this example is similar to that of example 1, except that: the component A comprises the following components in parts by weight:
6 portions of magnesium chloride
6 parts of high silica glass fiber
Zinc oxide 7.5 parts
Alkyd resin 30 parts
Magnesium hydroxy silicate 2 parts
Sodium bisulfate 2 parts
1-part of aluminum potassium sulfate
3 portions of expanded graphite powder
0.03 part of paraffin with 25 to 30 carbon atoms.
Comparative example 1
In the comparative example, hydrochloric acid pickling solution is adopted to clean the surface of the magnesium alloy ingot.
Comparative example 2
In the comparative example, the surface of the magnesium alloy ingot is cleaned by adopting the mixed alkaline washing liquor of sodium hydroxide, sodium bicarbonate and sodium carbonate.
Comparative example 3
In the comparative example, a commercially available organic cleaning agent was used to clean the surface of the magnesium alloy ingot.
The number of ingots cleaned in the above examples and comparative examples was 100, and the cleaning yield was as shown in the following table (the cleaning results were expressed as cleaning yields, and the results were passed without oil stains, flow marks, and debris on the surface of the ingot, and when one of the results was not satisfied, the result was regarded as a failure).
The cleaning method disclosed by the embodiment of the invention has the advantages that the coating layer with certain adsorption performance and oil removal performance is formed on the surface of the magnesium alloy ingot to be treated by utilizing the matching of special materials and the solidification characteristic of a high polymer material, and then the coating layer is torn off by utilizing the characteristic of easiness in separation between the coating layer and the magnesium alloy ingot body, so that the dirt on the surface of the magnesium alloy ingot is also removed while the coating layer is torn off, and meanwhile, the surface of the magnesium alloy ingot is not influenced.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the embodiments of the present invention and not for limiting the same, and although the embodiments of the present invention are described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the embodiments of the present invention, and these modifications or equivalent substitutions cannot make the modified technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (9)
1. A magnesium alloy ingot surface cleaning method is characterized by comprising the following steps:
step one, weighing raw materials according to the following components in parts by weight to prepare a component A:
4-6 parts of magnesium chloride
3-6 parts of high silica glass fiber
6-8 parts of zinc oxide
28-30 parts of alkyd resin
2-3 parts of magnesium silicate hydroxide
2-3 parts of sodium bisulfate
1-2 parts of aluminum potassium sulfate
3-4 parts of expanded graphite powder
0.02-0.03 part of paraffin with 25-30 carbon atoms
The preparation method of the alkyd resin comprises the following steps: mixing rice bran oil and n-butanol, heating to 115-120 ℃, dropwise adding a saturated lithium hydroxide solution as a catalyst, and continuously heating to 250 ℃ for reaction for 4-6 h; cooling to 120 ℃ after the reaction is finished, then adding phthalic anhydride and ethanol, heating to 160 ℃ for reaction for 4-6h after the reaction is finished, cooling to 50-60 ℃ after the reaction is finished, then dropwise adding mixed TDI and xylene, heating to 105 ℃ after the dropwise adding is finished, reacting for 6-8h, cooling to 50-60 ℃ after the reaction is finished, then adding ethylene glycol, keeping the temperature and stirring for 2-4h, then naturally cooling, and filtering to obtain the needed alkyd resin; in the first step, the mass ratio of rice bran oil, n-butanol, phthalic anhydride, ethanol, TDI, xylene and ethylene glycol in the alkyd resin preparation process is 1: (0.4-0.5): (0.2-0.3): (2-3): (0.2-0.25): (0.1-0.2): (0.08-0.15); the addition amount of the saturated lithium hydroxide solution is 1 drop per 5ml of reactants;
mixing the raw materials, grinding the mixture in a planetary grinder until the mixture is uniform and the size of the solid is less than 1 mu m to obtain a component A;
step two, uniformly mixing the component A and an alkyd resin curing agent to prepare a cleaning solution, immediately soaking a cast mother alloy ingot obtained after casting in the cleaning solution, and taking out the ingot after a coating layer is formed on the surface of the ingot;
the addition amount of the alkyd resin curing agent is 8-15% of the mass of the alkyd resin in the first step;
and step three, drying the surface of the cast ingot at the temperature of 80-100 ℃, and tearing off the solidified coating layer by using external force when the temperature is reduced to 30-40 ℃ after drying to obtain the master alloy cast ingot with the surface cleaned.
2. The method for cleaning the surface of a magnesium alloy ingot according to claim 1, characterized in that: in the first step, the granularity of magnesium chloride, zinc oxide, magnesium hydroxy silicate, sodium bisulfate, aluminum potassium sulfate and expanded graphite powder is 0.05-0.1 μm.
3. The method for cleaning the surface of a magnesium alloy ingot according to claim 1, characterized in that: in the first step, the length of the high silica glass fiber is 0.5-2mm, and the diameter is 15-20 μm.
4. The method for cleaning the surface of a magnesium alloy ingot according to claim 1, characterized in that: in the second step, the addition amount of the alkyd resin curing agent is 10-12% of the mass of the alkyd resin in the first step.
5. The method for cleaning the surface of a magnesium alloy ingot according to claim 1, characterized in that: in the second step, the thickness of the wrapping layer is 300-400 μm.
6. The method for cleaning the surface of a magnesium alloy ingot according to claim 1, characterized in that: in the third step, the drying time is 10-15 minutes.
7. The method for cleaning the surface of a magnesium alloy ingot according to claim 1, characterized in that: in the third step, the temperature is reduced to 3-4 ℃/s after drying.
8. The method for cleaning the surface of a magnesium alloy ingot according to claim 1, characterized in that: in the third step, the hardness of the dried coating layer is in the range of 2B-2H in terms of pencil hardness.
9. The method for cleaning the surface of a magnesium alloy ingot according to claim 1, characterized in that: in the third step, the hardness of the dried coating layer is HB, F or H in terms of pencil hardness.
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| CN101967630B (en) * | 2009-07-28 | 2012-07-25 | 中国科学院金属研究所 | Method for preparing catalyst layer on surface of magnesium and magnesium alloy by chemical plating of nickel and nickel-phosphorus alloy |
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