WO2013111708A1 - Composition d'agent de libération de matrice - Google Patents

Composition d'agent de libération de matrice Download PDF

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Publication number
WO2013111708A1
WO2013111708A1 PCT/JP2013/051106 JP2013051106W WO2013111708A1 WO 2013111708 A1 WO2013111708 A1 WO 2013111708A1 JP 2013051106 W JP2013051106 W JP 2013051106W WO 2013111708 A1 WO2013111708 A1 WO 2013111708A1
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WO
WIPO (PCT)
Prior art keywords
release agent
mold
agent composition
resin
thermosetting resin
Prior art date
Application number
PCT/JP2013/051106
Other languages
English (en)
Japanese (ja)
Inventor
幹典 鈴木
押本　康成
有 松木
茂 酒向
正昭 石黒
森　正至
直人 上坂
一正 安田
師岡　将義
Original Assignee
ユシロ化学工業株式会社
株式会社デンソー
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Filing date
Publication date
Application filed by ユシロ化学工業株式会社, 株式会社デンソー filed Critical ユシロ化学工業株式会社
Priority to US14/372,914 priority Critical patent/US20150057401A1/en
Priority to DE112013000661.8T priority patent/DE112013000661T5/de
Priority to CN201380006153.0A priority patent/CN104125868B/zh
Publication of WO2013111708A1 publication Critical patent/WO2013111708A1/fr

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22C—FOUNDRY MOULDING
    • B22C3/00—Selection of compositions for coating the surfaces of moulds, cores, or patterns
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21J—FORGING; HAMMERING; PRESSING METAL; RIVETING; FORGE FURNACES
    • B21J3/00—Lubricating during forging or pressing
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/04—Elements
    • C10M2201/041—Carbon; Graphite; Carbon black
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/06—Metal compounds
    • C10M2201/061—Carbides; Hydrides; Nitrides
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/06—Metal compounds
    • C10M2201/065—Sulfides; Selenides; Tellurides
    • C10M2201/066—Molybdenum sulfide
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/10—Compounds containing silicon
    • C10M2201/102—Silicates
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/10—Compounds containing silicon
    • C10M2201/102—Silicates
    • C10M2201/103—Clays; Mica; Zeolites
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2203/00—Organic non-macromolecular hydrocarbon compounds and hydrocarbon fractions as ingredients in lubricant compositions
    • C10M2203/10—Petroleum or coal fractions, e.g. tars, solvents, bitumen
    • C10M2203/1006—Petroleum or coal fractions, e.g. tars, solvents, bitumen used as base material
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2205/00—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions
    • C10M2205/14—Synthetic waxes, e.g. polythene waxes
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2205/00—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions
    • C10M2205/16—Paraffin waxes; Petrolatum, e.g. slack wax
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2205/00—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions
    • C10M2205/18—Natural waxes, e.g. ceresin, ozocerite, bees wax, carnauba; Degras
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2209/00—Organic macromolecular compounds containing oxygen as ingredients in lubricant compositions
    • C10M2209/10—Macromolecular compoundss obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • C10M2209/101—Condensation polymers of aldehydes or ketones and phenols, e.g. Also polyoxyalkylene ether derivatives thereof
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2209/00—Organic macromolecular compounds containing oxygen as ingredients in lubricant compositions
    • C10M2209/10—Macromolecular compoundss obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • C10M2209/102—Polyesters
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2217/00—Organic macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2217/04—Macromolecular compounds from nitrogen-containing monomers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • C10M2217/043—Mannich bases
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2217/00—Organic macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2217/04—Macromolecular compounds from nitrogen-containing monomers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • C10M2217/045—Polyureas; Polyurethanes
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2020/00—Specified physical or chemical properties or characteristics, i.e. function, of component of lubricating compositions
    • C10N2020/01—Physico-chemical properties
    • C10N2020/055—Particles related characteristics
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2040/00—Specified use or application for which the lubricating composition is intended
    • C10N2040/20—Metal working
    • C10N2040/24—Metal working without essential removal of material, e.g. forming, gorging, drawing, pressing, stamping, rolling or extruding; Punching metal
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2040/00—Specified use or application for which the lubricating composition is intended
    • C10N2040/20—Metal working
    • C10N2040/242—Hot working
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2040/00—Specified use or application for which the lubricating composition is intended
    • C10N2040/20—Metal working
    • C10N2040/244—Metal working of specific metals
    • C10N2040/245—Soft metals, e.g. aluminum
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2040/00—Specified use or application for which the lubricating composition is intended
    • C10N2040/36—Release agents or mold release agents

Definitions

  • the present invention relates to a release agent composition. More specifically, the present invention relates to a mold used for squeeze casting and low pressure casting of an aluminum alloy or the like, and a mold release agent composition used by applying to a mold used for die forging such as an aluminum alloy and steel. About.
  • a metal forming method using a metal mold there are a casting method and a die forging method, and examples of the casting method include a low pressure casting method and a die casting method.
  • a mold release agent is used for the purpose of suppressing the reaction (welding) between the mold and the molten metal before filling the mold with the molten metal and assisting the mold release of the molded product.
  • the squeeze die casting method which is one of the low pressure casting method and the die casting method
  • the filling speed of the molten metal such as an aluminum alloy into the cavity is small, so that the fluidity at the time of filling is ensured,
  • the mold temperature and the temperature of the molten metal are kept higher than the general high speed die casting method.
  • a mold release agent suitable for such high temperature forming what contains a powder is often used in order to obtain a heat insulation effect.
  • a coating agent composed of inorganic powder and water glass may be used.
  • an aqueous mold and an oil mold as a mold release agent.
  • a mold release agent is spray-coated on a mold before casting to form a film.
  • water is used as a dispersion medium, and a binder component such as an inorganic powder such as talc, a water-soluble polymer, a dispersant for dispersing the inorganic powder in water, Compositions containing organic compounds for the purpose of lubricating or preventing seizure such as wax and silicone have been used.
  • the oil-based mold release agent a composition obtained by diluting silicone oil with a solvent is used.
  • the dimensional accuracy is affected.
  • the release agent component is gasified.
  • problems such as being caught in products (such as castings) and causing internal defects. Therefore, in order to suppress the occurrence of such a problem, a measure of narrowing the discharge amount may be taken.
  • an aqueous release agent containing an inorganic lubricant, true spherical resin particles, and an organic carboxylic acid metal salt is known as a release agent containing powder and water as a dispersion medium.
  • a release agent containing powder and using an organic solvent as a dispersion medium a lubricant release agent containing a powdery solid lubricant, an adhesion improver, and a volatile solvent (see, for example, Patent Document 2).
  • a mold release agent for metal casting containing a solvent having a specific kinematic viscosity, an inorganic powder having a specific color tone, an inorganic powder such as graphite or carbon black is known. .
  • the water-based mold release agent containing powder accumulates on the mold with continuous use, and adversely affects the dimensional accuracy and product appearance, which necessitates regular cleaning work and lowers production efficiency. It is the cause.
  • the measure for reducing the deposition amount leads to a decrease in the adhesiveness (film forming property) of the release agent, it is not easy to achieve both suppression of deposition and film forming property. Further, in order to suppress excessive film formation, narrowing the discharge amount often causes clogging of the spray nozzle, particularly when the release agent contains powder.
  • the temperature of the mold is higher than 300 ° C., it has a film forming ability that sufficiently exhibits heat retention and releasability, and does not easily deposit on the mold and clog the spray nozzle. There is a need for mold release agents.
  • a coating agent may be used in the low pressure casting method, but there are problems such as a non-uniform film thickness and a rough surface of the cast due to a rough coating surface. Further, since the coating film becomes thinner with time, there is a problem that the dimensional accuracy of the product is lowered.
  • the present invention has been made in view of the above-described conventional situation, and is applied to a mold used for squeeze casting of aluminum alloy or the like and low pressure casting, and a mold used for die forging of aluminum alloy or steel or the like.
  • An object of the present invention is to provide a mold release agent to be used.
  • thermosetting resin having excellent heat resistance When a thermosetting resin having excellent heat resistance is used as the binder component in the release agent, a strong film is formed and the peelability of the film is improved by its thermal decomposition behavior. That is, by blending a predetermined amount of thermosetting resin, a strong film is formed in the process of film formation, and the film becomes brittle and easily removed after contact with high-temperature molten metal.
  • an oil-based mold release agent that uses mineral oil as a dispersion medium and using a solid lubricant as a mold release component, decomposition of the mold release agent is suppressed, and a sufficiently thick film is formed to maintain heat insulation. Property is also ensured, and a predetermined mold temperature can be maintained.
  • a mold release agent with better performance can be obtained by blending a polymer compound such as waxes according to the mold temperature. That is, when a solid lubricant and a thermosetting resin are dispersed in mineral oil and a wax is added thereto, a film can be formed in a short spray time even for a high-temperature mold exceeding 400 ° C. Production efficiency can be improved. On the other hand, when the mold tends to be excessively attached to a mold of 400 ° C. or lower, and the peelability of the film tends to decrease, other waxes or other polymer compounds excluding waxes, such as polybutene, etc. By using, high film forming ability is similarly exhibited without impairing the peelability of the film.
  • the solid lubricant can be sufficiently dispersed by performing a process such as high-speed stirring in the process of preparing the release agent, and can prevent clogging of the spray nozzle.
  • thermosetting resin has different viscosity and curing speed at the time of heat melting depending on the average molecular weight, and can obtain an adhesion force according to the average molecular weight. Therefore, by using a thermosetting resin having a predetermined average molecular weight depending on molding conditions such as molding method and mold temperature, a strong film can be formed at the time of molding, and the subsequent thermosetting resin The mold can be easily removed by thermal decomposition, and the release agent residue can be easily removed from the mold surface. Furthermore, by using a thermosetting resin having a predetermined average molecular weight, it is possible to obtain a release agent composition that exhibits characteristics that are unlikely to cause deposition on a mold and clogging of a spray nozzle. The present invention has been made based on such knowledge.
  • the present invention is as follows. 1. A release agent composition comprising a mineral oil or synthetic oil, a solid lubricant, a thermosetting resin, and a polymer compound, and applied to an inner surface of a casting or forging die. 2.
  • the solid lubricant is at least one selected from talc, boron nitride, graphite, mica, molybdenum disulfide, and fullerene.
  • the average particle size of the solid lubricant is 0.5 to 30 ⁇ m, and the total of the mineral oil or synthetic oil, the solid lubricant, the thermosetting resin, and the polymer compound is 100% by mass, 1.
  • the solid lubricant having a content of 1 to 10% by mass. Or 2.
  • thermosetting resin is at least one of phenol resin, epoxy resin, urea resin, melamine resin, alkyd resin, and unsaturated polyester resin. To 3. The mold release agent composition of any one of these. 5. The mold release agent composition according to any one of claims 1 to 4, wherein the thermosetting resin becomes a binder when the mold release agent composition is applied to a mold and decomposes at a molding temperature. . 6). 6. The adhesive force is 0.1 to 5.0 MPa when the number average molecular weight of the thermosetting resin is 5,000 to 500,000 and the molding temperature is 300 to 550 ° C. The mold release agent composition of any one of them. 7). 1. The polymer compound is at least one of synthetic wax and natural wax. To 6.
  • the polymer compound is at least one of synthetic wax and polybutene.
  • the polybutene is used when the mold temperature during coating is 250 ° C. or higher and lower than 400 ° C.
  • the synthetic wax is used when the mold temperature during coating is 400 ° C. or higher and 550 ° C. or lower.
  • the average molecular weight in this invention is the number average molecular weight of polystyrene conversion measured by the gel permeation chromatography.
  • the release agent composition of the present invention since it contains a mineral oil or synthetic oil, a solid lubricant, a thermosetting resin, and a polymer compound, even a high-temperature mold can be more quickly formed by a release agent component. A film is formed on the substrate, and the temperature drop of the mold is suppressed. In addition, since the film is easily decomposed by the heat of the mold and the molten metal during molding and the coating becomes brittle and the deposition of the release agent component is greatly reduced, a product having excellent dimensional accuracy and appearance can be obtained. . Furthermore, since the heat resistance of the release agent is high, it is possible to obtain a high-quality product with few internal defects such as a cast hole due to the decomposition gas of the release agent component.
  • the solid lubricant is at least one of talc, boron nitride, graphite, mica, molybdenum disulfide and fullerene
  • decomposition of the release agent component is sufficiently suppressed, and a coating having a predetermined thickness is formed. Since it can be formed and heat retention is ensured, a predetermined mold temperature can be maintained.
  • the average particle size of the solid lubricant is 0.5 to 30 ⁇ m and the total of the mineral oil or synthetic oil, the solid lubricant, the thermosetting resin, and the polymer compound is 100% by mass
  • the solid lubricant When the content of is 1 to 10% by mass, the powder particles are not agglomerated, clogging of the spray nozzle is suppressed, and unevenness of the coating surface due to coarse particles is also suppressed.
  • the thermosetting resin is at least one of phenol resin, epoxy resin, urea resin, melamine resin, alkyd resin, and unsaturated polyester resin, a sufficiently strong film is formed, Due to the thermal decomposition behavior of the film, the peelability of the coating is further improved.
  • thermosetting resin becomes a binder when the release agent composition is applied to the mold, it decomposes at the temperature at the time of molding, a strong film can be formed at the time of molding, and thereafter It can be easily demolded by decomposition, and the release agent residue from the mold surface can be easily removed.
  • the number average molecular weight of the thermosetting resin is 5,000 to 500,000
  • the molding temperature is 300 to 550 ° C.
  • the adhesive force is 0.1 to 5.0 MPa
  • the molding method By using a thermosetting resin having a predetermined average molecular weight depending on molding conditions and the like, a release agent composition having sufficient adhesion can be obtained.
  • the polymer compound is at least one of a synthetic wax and a natural wax
  • a film can be formed in a short spray time even on a high temperature mold exceeding 400 ° C., and the production efficiency. Can be improved.
  • the polymer compound is at least one of synthetic wax and polybutene
  • the mold temperature during coating is 250 ° C. or higher and lower than 400 ° C.
  • polybutene is used
  • the temperature of the mold is set. Regardless, the coating can be easily formed in a short spray time.
  • FIG. 1 It is explanatory drawing showing the outline of the apparatus used for the discharge of the mold release agent composition for forming a film, and the air blow for removing the formed film.
  • A is explanatory drawing showing a mode that spray-releases a mold release agent toward a steel plate and forms a film, (b) imitates a type
  • (A) is explanatory drawing showing a mode that spray-releases a mold release agent composition toward a steel plate, and forms a film, (b) mounts a metal cylinder on a film imitating a type
  • FIG. 5 is an explanatory view showing a state in which molten aluminum is supplied into the cylinder
  • (c) is an explanatory view showing a state in which the metal cylinder and the disk-shaped formed body are removed from the coating
  • (d) are explanatory drawings showing a mode that the film is removed by air blow. It is explanatory drawing of the test piece for measuring a fracture shear stress.
  • (A) is a schematic diagram of the cross section and plane of the iron plate before joining
  • (b) is a schematic diagram of the cross section and plane of the joined iron plate
  • (c) is the tensile direction of the two iron plates joined. It is a schematic diagram showing.
  • the release agent composition of the present invention contains mineral oil or synthetic oil, a solid lubricant, a thermosetting resin, and a polymer compound. Moreover, it is applied to the inner surface of a casting or forging die.
  • the mineral oil or synthetic oil used as the dispersion medium is not particularly limited.
  • various mineral oils can be used, for example, turbine oil described in JIS K 2213, gear oil described in JIS K 2219, machine oil described in JIS K 2238, and the like. Can be mentioned.
  • synthetic oil various oils such as polyalphaolefin, polyester, and polyglycol can be used.
  • the kinematic viscosity at 40 ° C. measured according to JIS K 2283 is 10 to 400 mm 2 / s, particularly 10 to 250 mm 2 / s, and further 10 to 100 mm 2 / s.
  • the mineral oil or synthetic oil which is s is preferable. Further, the blending amount of the mineral oil or synthetic oil is 75 to 90% by mass, particularly 80 to 85% when the total amount of the mineral oil or synthetic oil, solid lubricant, thermosetting resin and polymer compound is 100% by mass. It is preferable that it is mass%.
  • the solid lubricant is not particularly limited, and examples thereof include talc, boron nitride, graphite, mica, molybdenum disulfide, and fullerene.
  • the solid lubricant preferably has an average particle size of 30 ⁇ m or less, particularly 0.5 to 30 ⁇ m, from the viewpoint of preventing nozzle clogging during spray coating.
  • the blending amount of the solid lubricant is 1 to 10% by mass, particularly 3 to 7% by mass, when the total amount of mineral oil or synthetic oil, solid lubricant, thermosetting resin and polymer compound is 100% by mass. % Is preferred.
  • the aggregated particles of the solid lubricant cause clogging of the nozzle during spray coating, and if the aggregated particles are applied as they are, coarse particles will be present in the coating, resulting in irregularities on the surface of the molded product. Problems occur. Therefore, it is preferable to sufficiently disperse the solid lubricant by a mechanical treatment using a high-speed stirrer, a colloid mill or the like when preparing the release agent composition.
  • thermosetting resin is not particularly limited, and examples thereof include phenol resin, epoxy resin, urea resin, melamine resin, alkyd resin, and unsaturated polyester resin.
  • a thermosetting resin By containing a thermosetting resin, a strong film can be formed.
  • the thermosetting resin has high performance as a binder and also improves the peelability of the film by thermal decomposition after molding.
  • the average molecular weight of the thermosetting resin is preferably 6,000 to 1,000,000. In order to obtain a particularly strong adhesive force, the average molecular weight is preferably 6,000 to 100,000. In order to easily peel at the time of demolding, the average molecular weight exceeds 100,000, and 1,000,000. The following is preferable.
  • the average molecular weight of the thermosetting resin is set in consideration of adhesion and peelability.
  • the blending amount of the thermosetting resin is 1 to 15 when the total amount of mineral oil or synthetic oil, solid lubricant, thermosetting resin and polymer compound is 100% by mass from the viewpoint of improving the peelability. It is preferably 2% by mass, particularly 2 to 12% by mass, and more preferably 3 to 7% by mass.
  • polymer compound examples include synthetic waxes such as paraffin wax, polyethylene wax, polypropylene wax, oxidized polyethylene wax and oxidized polypropylene wax, natural waxes such as beeswax, carnauba wax and montan wax, and polybutene and polyalkylene glycol. Can be mentioned.
  • synthetic waxes such as paraffin wax, polyethylene wax, polypropylene wax, oxidized polyethylene wax and oxidized polypropylene wax, natural waxes such as beeswax, carnauba wax and montan wax, and polybutene and polyalkylene glycol.
  • the compounding amount of the polymer compound is 2 to 15% by mass, particularly 2 to 10% by mass, when the total amount of mineral oil or synthetic oil, solid lubricant, thermosetting resin and polymer compound is 100% by mass. %, Preferably 4 to 8% by mass.
  • the polymer compound synthetic wax, polybutene and the like are preferable, and as the synthetic wax, paraffin wax, oxidized polyethylene wax, oxidized polypropylene wax, particularly paraffin wax and oxidized polyethylene wax are preferable.
  • the polymer compound is preferably used depending on the temperature of the mold.
  • synthetic waxes such as paraffin wax and polybutene are used as the polymer compound, and when the mold temperature when applying the release agent is 250 ° C. or more and less than 400 ° C., polybutene is used, and the mold when applying the release agent.
  • the temperature is 400 ° C. or higher and 550 ° C. or lower, it is particularly preferable to use a synthetic wax such as paraffin wax. In this way, a film having a predetermined thickness can be easily formed in a short spray time regardless of the temperature of the mold.
  • a lubricant other than the above-described solid lubricant can be contained as a lubricant component.
  • Other lubricants are not particularly limited, and examples thereof include silicone compounds, fats and oils, other synthetic oils excluding the synthetic oils used as the dispersion medium, and inorganic powders.
  • the silicone compound may be an organopolyester partially or wholly modified with an alkyl group, aralkyl group, carboxylalkyl group or carboxylate alkyl group, hydroxyalkyl group, aminoalkyl group, or the like. Siloxane or the like can be used.
  • lubricants include the above-mentioned various lubricants, fats and oils such as animal and vegetable oils, polyester-based synthetic lubricants, ZnDTP, MoDTP, ZnDTC, MoDTC, phosphorus-based and sulfur-based extreme pressure additives, calcium Sulfonates can be used. Furthermore, in addition to these lubricants, any lubricant that is usually used in a die casting mold release agent can be used without particular limitation.
  • the blending amount of the other lubricant is preferably 1 to 10 parts by mass when the total amount of mineral oil or synthetic oil, solid lubricant, thermosetting resin and polymer compound is 100 parts by mass.
  • the film formed using the release agent composition can have a thickness of 2 to 20 ⁇ m, preferably 3 to 15 ⁇ m, particularly preferably 5 to 10 ⁇ m. If the thickness of the coating is less than 2 ⁇ m, problems may occur in lubricity, heat retention and releasability, and sufficient performance as a release agent may not be exhibited. On the other hand, if the thickness of the coating exceeds 20 ⁇ m, the releasability is lowered, the residue of the release agent component is easily deposited on the mold surface, and the release agent component and its decomposition product are mixed into the molded product. Sometimes, it is not preferable.
  • the coating amount of the release agent composition depends on the mold shape and the like, but in order to make the thickness of the film in the above-mentioned range, the area of the inner surface of the mold is usually 0.004 m 2 . It is about 0.07 to 0.17 cm 3 , particularly about 0.10 to 0.14 cm 3 .
  • the method for forming a film on the surface of the mold and the method for removing the film after production of the molded body and after molding are not particularly limited. For example, using a device such as FIG. However, as shown in FIGS. 2 and 3, it is possible to form a film, produce a molded body, and remove the film.
  • the spray nozzle used at the time of film formation is not particularly limited, an external mixing type two-fluid mixing nozzle such as the two-fluid mixing nozzle 1 with a needle valve in FIG. 1 can be used.
  • a pipe b is connected to a compressor, and pressurized air from the compressor is sent to three pipes at a connector 6.
  • the piping 63 is provided with a pressure control valve 34 and a pressurized tank 4 containing a release agent composition.
  • a pressure control valve 32 and a port solenoid valve (electromagnetic valve) 22 are disposed in the pipe 61.
  • a pressure control valve 33 and a port solenoid valve 23 are disposed in the pipe 62.
  • the release agent adjusted to a predetermined pressure in the pressurized tank 4 is supplied from the pipe 63 to the two-fluid mixing nozzle 1 with a needle valve, and is fed into the pipe 61. Then, air (spraying air) having a predetermined pressure and a predetermined flow rate is sent in. Further, the solenoid valve control timer 5 is operated from the pipe 62 for a preset time, whereby the port solenoid valve 23 is operated and air (control air) is supplied. The needle valve is operated by the air (control air), and the release agent supplied from the pipe 63 and the air supplied from the pipe 61 are discharged and mixed at the nozzle tip only while the needle valve is operating. . At the same time, the mixed release agent component and air adhere to the mold to form a film. Thereafter, a molten metal such as an aluminum alloy is supplied into the mold, and after cooling, the mold is removed to produce a molded product.
  • a molten metal such as an aluminum alloy is supplied into the mold, and after cooling,
  • the pipe a is connected to a compressor, and pressurized air from the compressor is adjusted by the pressure control valve 31 and the flow rate is adjusted by the port solenoid valve 21.
  • the pressurized air whose pressure has been adjusted and whose flow rate has been adjusted is blown toward the coating from the air blowing nozzle 40 [see FIG. 3 (d)] connected to the pipe c, and the release agent component remaining on the mold surface and The decomposition products are removed and then these steps are repeated.
  • the steel plate 7 and the cylindrical jig 20 were used to simulate a mold.
  • the apparatus as shown in FIG. 1 was used for discharging the release agent composition for forming a film and for air blowing for removing the film after molding.
  • Examples 1 to 10 [1] Preparation of mold release agent composition Mineral oil (kinematic viscosity 20 mm 2 / s at 40 ° C.
  • the thickness of the coating varies considerably depending on the type and blending amount of the solid lubricant, thermosetting resin and polymer compound. Therefore, the thickness of the coating can be adjusted to a predetermined thickness in consideration of the molding conditions such as the type of molten metal, the temperature, the peelability of the coating after molding, and the like.
  • Example 4 there is a difference of 45 ° C. from the lowest temperature of 430 ° C. in Examples 1 and 10 to the highest temperature of 475 ° C. in Example 4, and the heat retaining performance depends on the composition of the release agent composition. It can be seen that there is a considerable difference. Therefore, the composition of the release agent composition can be set in consideration of other performance such as adhesion and peelability.
  • the evaluation results of the peelability were A evaluation for those that could be easily removed from the entire surface, and the portions that were in contact with the molten metal could be easily removed, but the portions that were not in contact were compared with the A evaluation. Those that required a longer time were evaluated as B, and those that required longer time than the B evaluation for both the portion that was in contact with the molten metal and the portion that was not in contact were rated as C. The results are listed in Table 5.
  • Example 6 using a synthetic wax as a polymer compound, graphite as a solid lubricant, a phenol resin as a thermosetting resin, and Example 7 using a urea resin as a thermosetting resin together with a synthetic wax and graphite, It has excellent peeling performance regardless of the steel plate temperature, and it can be seen that these release agent compositions can be used without considering the temperature of the steel plate.
  • thermosetting resins Examples 11 to 18 Mineral oil used in Example 1 as a mineral oil, wax used in Example 1 as a polymer compound, boron nitride used in Example 5 as a solid lubricant, and four types of phenol resins having different average molecular weights as thermosetting resins, A release agent composition was prepared in the same manner as in Example 1 using two types of melamine resins having different average molecular weights, diallyl phthalate resin, and urea resin. Moreover, in the above-described evaluation of the adhesion performance, the upper limit temperature of the mold temperature at which the film thickness is 10 ⁇ m or more was evaluated as the upper limit temperature for adhesion. Furthermore, in the evaluation of the film peeling performance, the lower limit value of the mold temperature that becomes A evaluation or B evaluation was evaluated as the peelable lower limit temperature. The results are listed in Table 6.
  • the usable mold temperature range varies depending on the type of thermosetting resin.
  • the mold temperature at which the release agent is used For example, when the product temperature is inevitably high due to the thick product thickness, it is preferable to use the phenol resins of Examples 13 and 14 having a large average molecular weight.
  • the mold temperature is lowered, such as when cooling is strengthened to shorten the molding cycle time, it is preferable to use the urea resin of Example 18.
  • the adhesion performance and the peeling performance can be made compatible with each mold temperature.
  • Example 19 to 26 Mineral oil used in Example 1 as a mineral oil, wax used in Example 1 as a polymer compound, boron nitride used in Example 5 as a solid lubricant, and phenol resin as a thermosetting resin, Example 1
  • a release agent composition was prepared.
  • the phenol resin four types of resins having different average molecular weights used in Examples 11 to 14 were used. Specifically, the number average molecular weights are 6000 (Examples 19 and 23), 10,000 (Examples 20 and 24), 45,000 (Examples 21 and 25), and 300,000 (Examples 22 and 26). 4), a test piece as shown in FIG.
  • the material of the two iron plates Fa and Fb used for the production of the test piece of FIG. 4 is SUS304, and the dimensions are 35 mm in length, 10 mm in width, and 2 mm in thickness.
  • the phenol resin layer P formed on one end of the iron plate Fa has a length of about 10 mm, a width of about 10 mm, and a thickness of about 0.2 mm [see FIG. 4A].
  • one end of an iron plate Fb heated to 350 ° C. or 500 ° C. is placed on the phenol resin layer P of the iron plate Fa at room temperature (25-30 ° C.), and then naturally cooled to room temperature. Produced.
  • breaking shear stress was measured by sandwiching the other end of each of the iron plates Fa and Fb with a chuck of a tensile tester and pulling it in the direction of the arrow in FIG. 4C at a tensile speed of 0.1 mm / second. .
  • thermosetting resin e.g., phenolic resin
  • Viscosity increases, and it becomes difficult to spread on the mold surface.
  • an average molecular weight increases, so that an average molecular weight is large, it is thought that it becomes difficult to spread on the mold surface more.
  • the larger the average molecular weight the smaller the bonding area and the shorter the curing time, the insufficient adhesive force is not expressed, and the fracture shear stress that serves as an index of adhesion tends to decrease.
  • thermosetting resin since the thermosetting resin was sprinkled as a single resin, there may be a difference from when sprinkled as a release agent composition containing other components.
  • Table 7 and FIG. 6 as the average molecular weight of the phenol resin is increased, the adhesion area ratio is decreased, and the fracture shear stress is also decreased at the same time. I understand.
  • the adhesion area ratio means [(actually adhered area) / (area sprinkled with phenol resin powder)] ⁇ 100.
  • the temperature is 350 ° C.
  • the average molecular weight is 45,000, it is assumed that the curing is slowed, the viscosity is lowered, the adhesion area ratio is increased, and the fracture shear stress is increased.
  • the average molecular weight is 300,000, the curing is slow, but the viscosity is originally high, so the adhesion area ratio does not increase, and the fracture shear stress is estimated to be slightly increased.
  • thermosetting resins except a phenol resin. That is, it is considered that not only the phenol resin but also other thermosetting resins such as melamine resin and urea resin have the same tendency, and the type of thermosetting resin depends on molding conditions such as molding method and mold temperature.
  • the present invention can be used in the technical field of metal molding.
  • it can be utilized in technical fields such as low-pressure casting and squeeze casting of aluminum alloys and die forging.

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Mold Materials And Core Materials (AREA)
  • Moulds For Moulding Plastics Or The Like (AREA)
  • Lubricants (AREA)
  • Application Of Or Painting With Fluid Materials (AREA)
  • Forging (AREA)

Abstract

La présente invention se rapporte à une composition d'agent de libération de matrice qui est utilisée en étant enduite sur une matrice utilisée pour le forgeage en matrice ou une matrice utilisée pour le moulage de métal ou le moulage basse pression. Composition d'agent de libération de matrice contenant : une huile minérale ou une huile synthétique ; un lubrifiant solide (par exemple, du talc, du nitrure de bore, du plomb noir, du mica ou du bisulfure de molybdène dont les particules ont de préférence un diamètre moyen entre 0,5 et 30 μm et dont la teneur est comprise entre 1 et 10% en masse) ; une résine thermodurcissable (différentes résines, telles que la résine de mélanine, résine d'urée, et résine de phénol ayant des poids moléculaires moyens différents peuvent être sélectionnées et utilisées en fonction de la force d'adhérence nécessaire) ; et un composé polymère (par exemple, une cire synthétique ou du polybutène). Ledit agent de libération de matrice est utilisé en étant enduit sur la surface interne d'une matrice de forgeage ou de moulage.
PCT/JP2013/051106 2012-01-23 2013-01-21 Composition d'agent de libération de matrice WO2013111708A1 (fr)

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DE112013000661.8T DE112013000661T5 (de) 2012-01-23 2013-01-21 Formlösemittelzusammensetzung
CN201380006153.0A CN104125868B (zh) 2012-01-23 2013-01-21 脱模剂组合物

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DE112013000661T5 (de) 2014-11-13

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