CN114045053A - Decarburization-preventing separant - Google Patents

Decarburization-preventing separant Download PDF

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CN114045053A
CN114045053A CN202111420583.XA CN202111420583A CN114045053A CN 114045053 A CN114045053 A CN 114045053A CN 202111420583 A CN202111420583 A CN 202111420583A CN 114045053 A CN114045053 A CN 114045053A
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parts
powder
weight
decarbonization
coating
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谢家鼎
顾红霞
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Shanghai Moser Science And Technology Co ltd
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Shanghai Moser Science And Technology Co ltd
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING 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
    • C09D1/00Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances
    • C09D1/02Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances alkali metal silicates
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D5/00Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/20Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes for coatings strippable as coherent films, e.g. temporary coatings strippable as coherent films
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING 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
    • C09D7/00Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40Additives
    • C09D7/60Additives non-macromolecular
    • C09D7/61Additives non-macromolecular inorganic
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING 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
    • C09D7/00Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40Additives
    • C09D7/70Additives characterised by shape, e.g. fibres, flakes or microspheres

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  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
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  • Inorganic Chemistry (AREA)
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Abstract

The invention discloses an anti-decarbonization separant, which comprises the main raw materials of 10-38 parts by weight of mullite powder, 10-20 parts by weight of sepiolite powder and Al2O310 to 25 parts by weight of Cr2O310-25 parts by weight of SiC 10-25 parts by weight, 8-20 parts by weight of binder and 30-50 parts by weight of water. According to the invention, a melt film shielding protection mechanism and an oxidation reduction protection mechanism are combined, resources of sepiolite and mullite powder are fully utilized, the sepiolite and the mullite powder are mixed and added into a formula of the decarburization-preventing separant, and the prepared decarburization-preventing separant has a good antioxidation and decarburization-preventing effect; the physical mechanical property and the chemical property of the protected high-speed steel are not influenced; the cleaning is convenient and the peeling is automatic after the use and heating.

Description

Decarburization-preventing separant
Technical Field
The invention relates to the field of metal coatings, in particular to an anti-decarbonization separant.
Background
When the metal is heated, the workpiece is exposed to air, and oxidation and decarburization (i.e., reduction in carbon content on the surface of the steel part) often occur, which adversely affect the surface properties of the heat-treated part. In particular, in the manufacturing process of steel products, the fuel adopted in the hot rolling process of high-speed steel is coal, coke or natural gas, the temperature is up to 1280 ℃, and oxidizing substances such as O, CO, SO and the like exist in the heating atmosphere, SO that the high-speed steel is inevitably subjected to chemical corrosion, and the main expression forms of the chemical corrosion are oxidation and decarburization. In actual production, in order to remove the oxide scale and the decarburized layer, surface layer removing treatment is required, which is labor-consuming and time-consuming, and greatly influences the economic benefit of enterprises. The oxidation and decarburization in the rolling process is a technical problem which troubles related enterprises.
On one hand, the oxygen-less and non-oxidation heating of the steel can be realized through automatically adjusting the fuel gas components of the heating furnace, salt bath heating, rapid heating and vacuum protection. However, since the investment cost of equipment is high and mass production is not facilitated, the large-scale production cannot be performed. On the other hand, protective heating may also be performed using paint or packaging methods. From the viewpoint of using method and economy, the anti-decarbonization and anti-oxidation coating technology which is easier to popularize at present forms a coating on the surface of a billet by controlling the element components in a high-temperature anti-oxidation coating system. At high temperature, the components in the coating react to form a uniform and compact adhesion layer on the surface of the billet steel to prevent oxygen from contacting with carbon, thereby achieving the purpose of preventing the oxidation and decarburization of the billet steel.
The protection mechanism of the coating is mainly divided into the following mechanisms: a melt film shielding type protection mechanism, a reaction type protection mechanism, a redox type protection mechanism and an inorganic layered barrier action mechanism. Through the protection mechanisms, corresponding high-temperature protection coatings can be developed to effectively protect the steel billet. The molten film shielding type protection mechanism refers to adhering a dense and stable glass-like material formed by a coating layer and a glass ceramic-like material to a metal surface layer upon high-temperature heat treatment, thereby blocking collision between gas and metal and achieving the intended protection purpose. The coating is prepared by mixing binder and glass frit, glass ceramic material, metal powder and other solvents with different crystal grain sizes at normal temperature, stirring to form paste colloid state, and coating the paste colloid on the surface of the material by brushing or spraying to form a protective layer with a certain thickness on the surface of the matrix. The redox protection mechanism is that reducing components are added into coating raw materials, and at a higher temperature, the components in the coating firstly react with oxidizing components in the atmosphere, a protective layer is generated, the oxygen content around the surface layer of a billet is reduced, and then the protection effect is realized. The reactive protection mechanism is that the coating is adhered to the steel surface layer, and when the steel surface layer is heated to a sufficient temperature, a small number of oxides on the steel surface layer are melted due to the action of the coating, the temperature is continuously increased, the oxides and the components in the coating are subjected to chemical transformation to generate a thin semi-molten melt film which is dispersedly and stably covered on the metal surface layer, so that the contact insulation between the atmosphere and the material surface is realized, and the protection of the substrate in the heating process is met. The inorganic layered barrier mechanism comprises a layered sheet structure, the inorganic melt can affect the structure to cause the layer spacing to be enlarged, and the inorganic melt can generate an intercalation effect with a layered matrix to obtain a nano two-dimensional layered structure, wherein different components exist at the same time.
Chinese patent CN 105177249A discloses an anti-decarbonization coating, which is composed of Na2O、SiO2、Al2O3、Cr2The composition O adopts cheaper industrial raw materials, has reasonable formula and good high-temperature resistance, and can greatly reduce the oxidation and decarbonization during heat treatment. CN 106566295A discloses a low-cost anti-decarbonization coating material for heavy rail steel and an application thereof, wherein the coating material comprises the following raw materials in percentage by weight: 43-52% of river sand and Al2O38-15% of powder and B2O310-15% of powder, 2-5% of light-burned dolomite, 12-17% of iron oxide red powder and Na21-2% of O powder and 8-11% of LF refining slag, and the anti-decarbonization coating material can effectively avoid surface decarbonization of a heavy rail steel casting blank in the heating process for a long time and reduce the depth of a decarbonization layer on the surface of the casting blank; after the anti-decarbonization coating material is adopted, the heavy rail steel casting blank is heated in a heating furnace with the oxygen content of furnace gas being more than or equal to 3% for 10-12 hours, the depth of a surface decarbonization layer is less than or equal to 0.4mm, and the relevant requirements of TB/T2344-12 are met; meanwhile, compared with the traditional anti-decarbonization coating material, the preparation cost of the coating material can be effectively reduced, the low-cost production of heavy rail steel products is realized, and the production cost per ton of steel is reduced by about 20 yuan.
However, in the prior art, the effect is not ideal often by adopting a single protection mechanism, the coating of the molten film shielding type protection mechanism cannot meet the protection requirement when the temperature is not high enough, and the problem that the coating is difficult to fall off and remove at the later stage exists, so that more time and money costs are spent, and therefore, the preparation of the separant which can effectively prevent decarburization in the production process of the steel piece, can automatically fall off after heating is finished, and has a simple preparation process and low cost is particularly important.
Disclosure of Invention
In order to solve the technical problems, the invention provides an anti-decarbonization release agent, which has the technical scheme that:
an anti-decarbonization separant comprises the following raw materials: mineral powder, Al2O3、Cr2O3SiC, binder and water.
The main component of sepiolite is SiO2MgO, etc., which are indispensable in typical high-temperature oxidation-preventing coatings, and which also have good plasticity, rheology, chemical inertness and thermal stability. The sepiolite has certain binding power, and has small shrinkage and difficult cracking after being dried, and the excellent performances show that the sepiolite can be used as powder of high-temperature anti-oxidation and anti-decarbonization coating, and one of the most important characteristics of the sepiolite is that high-viscosity suspension can be formed at quite low concentration. The fine fibrous crystal morphology allows the sepiolite to disperse well under applied pressure (system shear) and the crystals in solution are more influenced by gravity than by electrical properties, thus forming a random network of fibres in the trapped liquid, the suspension being characterized by non-newtonian flow. Its properties depend on the concentration of sepiolite, the magnitude of the shear force and the pH value. And the sepiolite colloidal suspension is little influenced by salt, the suspension does not flocculate and precipitate in dielectric medium, and other electrolytes such as ammonia water, sodium hydroxide, potassium chloride and inorganic phosphate also have little influence on the sepiolite.
Mullite belongs to silicate minerals, has a special crystal structure so as to have better high-temperature resistance, mullite powder is an aluminum silicate refractory material, and the main component is Al2O3And SiO2And small amounts of other components, e.g. Fe2O3、Na2O、K2O、CaO、MgO2、TiO2And the like. Both the mullite and the sepiolite have the feasibility of preparing the high-temperature anti-oxidation and anti-decarbonization coating, and the mullite powder and the sepiolite have rich resources and low price. Is more suitable for being developed into steel high-temperature heat treatment protective coatingAnd (5) feeding.
Most of the coating preparation uses the principle of eutectic melting, and powder with single component can not achieve the protection effect required by the coating, so that raw materials with multiple components are required to be selected as a coating base material, and then other raw materials are added to prepare a better protection coating. The invention fully utilizes the excellent performances of mullite and sepiolite and the characteristic of abundant resources, combines a melt film shielding type protection mechanism and an oxidation reduction protection mechanism, properly adds some auxiliary materials, and uses a slurry method to prepare the high-temperature anti-oxidation and anti-decarbonization coating. The most common basic raw materials in the design of high-temperature inorganic oxidation-resistant coatings are silicon oxide, aluminum oxide, magnesium oxide and chromium oxide, and the oxide system is also the basis of ceramic and glass industries and is the most familiar high-temperature material.
Since the sepiolite component of the present invention already contains a certain amount of MgO, no MgO is added to the coating in this patent. Adding a proper amount of Al into the coating2O3Can reduce the sintering temperature, promote the sintering of powder and form a compact coating. Meanwhile, the temperature of the liquid phase of the coating is reduced, powder particles are wetted and are close to each other, and air holes are filled. Finally, a compact protective layer is formed to isolate the contact of gas and the steel substrate.
Al2O3The refractory oxide is a refractory oxide material with high melting point, is widely used and cheap, and has good chemical stability, high mechanical strength and strong cold and hot shock resistance. At 1705-1815 ℃, the alumina resists the action of various gases and is stable in an oxidizing atmosphere and a strong reducing atmosphere. During melting of the coating, Al2O3Usually, free oxygen can be captured to form four coordination to enter a silica network, so that the glass network structure is strengthened, and the performance of the coating can be obviously improved, such as the chemical stability, hardness and elasticity of the coating are improved, the expansion coefficient of the coating can be reduced, the chemical activity of the coating is reduced, and the cracking of the surface of the coating can be prevented.
The melting point of the chromium oxide is 2277-2432 ℃. When volatilized, Cr2O3The oxygen in (1) is not lost due to the presence of CO or O2The rate of gasification under the atmosphere is constant. Under a strong reducing atmosphere, Cr2O3Will be reduced to metallic chromium, and chromium and Cr2O3A low temperature eutectic is formed at about 1594 ℃. Cr (chromium) component2O3And is resistant to most corrosive halides at high temperatures. Chromium oxide is commonly used in high temperature coatings of metal alloys and is used in large quantities.
SiC can react with oxygen at a lower temperature to generate SiO2,SiO2The membrane plays a certain role in preventing oxidation. By adding SiC by using a redox protection mechanism, the coating can firstly react with oxidizing gas before the coating reaches a sintering state, so that the contact between the coating and a steel matrix is reduced, and the protection effect of the coating at a low-temperature stage is enhanced. And SiC is a compound with extremely strong covalent bonds, can still maintain high bonding strength at a high temperature, has insignificant strength reduction, good thermal conductivity and small thermal expansion coefficient, and is considered to be an excellent high-temperature structural material and refractory material.
Further, the anti-decarbonization isolating agent comprises the following raw materials: mullite powder, sepiolite powder, Al2O3、Cr2O3SiC, binder and water.
Preferably, the binder is K2SiO3
The coating is a solid-liquid phase assembly. The solid phase is fine powder, and the mixing method of the solid phase and the liquid phase is different, and the effect is different. For water-based paints, the result of the paint formed by adding the carrier liquid to the powder is similar to that of the paint formed by adding the powder to the carrier liquid, but the effect is different, and in addition, the type and amount of the carrier liquid also have a certain influence on the overall effect of the paint. The invention selects water as the carrier liquid of the coating. Water is a good solvent, is safe and applicable, has rich sources and low price. The organic solvent is very volatile, has high price, causes pollution and is easy to burn at high temperature.
Further preferably, the anti-decarbonization isolating agent comprises the following raw materials in parts by weight: 10-38 parts of mullite powder, 10-20 parts of sepiolite powder and Al2O310 to 25 parts of Cr2O310-25 parts of SiC 10-25 parts, K2SiO38-20 parts of water and 30-50 parts of water.
The Al is2O3、Cr2O3The SiC is fine powder, the purity is more than 99%, and the particle sizes are respectively 500-1000 meshes independently.
The invention also provides a preparation method of the anti-decarburization release agent, which comprises the following steps:
s1 weighing the raw materials according to the formula, mixing mullite powder, sepiolite powder and Al2O3、Cr2O3Mixing SiC evenly to obtain mixed powder;
s2 reaction of K2SiO3Mixing with water, and stirring at 200-300 rpm for 5-10 min to obtain potassium silicate aqueous solution;
s3, adding the mixed powder obtained in the step S1 into the potassium silicate aqueous solution obtained in the step S2, and stirring at the rotating speed of 500-600 rpm for 15-20 min to obtain a mixed coating;
s4, standing the mixed coating prepared in the step S3 at room temperature for 30-60 min to obtain the decarburization isolating agent.
When the formula design of the high-temperature anti-oxidation coating is carried out, a protection mechanism is mainly used as a design basis, and generally, the high-temperature melting to form a compact film to isolate the contact between the furnace atmosphere and a metal matrix is the basis of the formula design. However, the invention adopts the combination of a melt film shielding type protection mechanism and an oxidation reduction protection mechanism, fully utilizes the resources of sepiolite and mola powder, and mixes the sepiolite and the mola powder and adds the sepiolite and the mola powder into the formula of the decarburization-preventing separant. When the separant prepared by the method is used in a low-temperature stage, substances such as silicon carbide powder and the like firstly react with oxygen, so that the oxygen potential near a coating film is reduced, and a matrix is protected from being oxidized; as the temperature rises, high-melting point oxides such as alumina, silicon carbide and mullite powder are used as frameworks, then the high-viscosity suspension formed by the sepiolite powder enables the framework substances to be fully dispersed, a disordered fiber network is formed in the trapped liquid, the contact between the heating atmosphere and a matrix is isolated, the protection effect in a high-temperature stage is achieved, and the protection effect of the protection coating is achieved in a wide temperature range.
In addition, when the coating is in a low-temperature stage, silicon carbide and oxygen react to generate silicon oxide, so that the oxygen potential is reduced; SiO 22Reacting with ferric oxide on the surface of the steel part at high temperature to generate a ceramic layer (fayalite) which is easy to peel off; al (Al)2O3The chemical stability is high, and the heat resistance of the coating can be improved; cr (chromium) component2O3Sepiolite powder and mullite powder increase the melting temperature of the glass enamel, rendering the coating inert to certain steels and allowing the coating to self-peel off as the workpiece cools. Compared with the prior art, the invention has the following beneficial effects:
1) the film is grayish green, the film is fast to form, the back surface of the film is smooth and clean, and the leveling property is good;
2) a layer of compact firm protective film capable of isolating the matrix from the heating atmosphere is formed on the surface of the metal during heating, so that the oxidation and decarburization phenomena of the high-speed steel are rapidly reduced, and other elements can be prevented from permeating into the steel;
3) the physical mechanical property and the chemical property of the protected high-speed steel are not influenced;
4) the cleaning is convenient after the use and heating, and the peeling is automatic;
5) no sagging occurs at high temperature, and no toxic gas is generated;
6) the coating has high adhesive force after coating, and has good stripping performance after heating.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below. The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention. The operations referred to in the examples are, unless otherwise specified, all those of ordinary skill in the art.
Some raw material parameters in the comparative examples and examples of the invention are as follows:
multo powder, available from Zheng State over sail refractory Limited;
sepiolite powder purchased from processing plants of shenghuang mineral products in Lingshou county;
Al2O3technical grade, particle size 500 mesh, available from 28095j, science and technology ltd, a new materials of fusion, zhou;
Cr2O3technical grade, particle size 500 mesh, available from 28095j, science and technology ltd, a new materials of fusion, zhou;
SiC, technical grade, particle size 500 mesh, available from 28095, science and technology, Inc., a material of fused New York, China.
Example 1
The preparation method of the anti-decarbonization release agent comprises the following steps:
s1 is prepared from mullite powder 30 weight portions, sepiolite powder 20 weight portions, and Al2O315 parts by weight of Cr2O3Mixing 18 parts by weight of SiC21 parts by weight to obtain mixed powder;
s2 weighing 16 parts by weight of K2SiO3Adding the mixture into 45 parts by weight of water, stirring at 200rpm for 5min, and uniformly mixing to obtain a potassium silicate aqueous solution;
s3, adding the mixed powder obtained in the step S1 into the potassium silicate aqueous solution obtained in the step S2, and stirring by using an electric stirrer at the rotating speed of 600rpm for 15min to obtain a mixed coating;
s4, standing the mixed paint prepared in the step S3 at room temperature for 60min to obtain the decarburization-preventing parting agent.
Comparative example 1
The preparation method of the anti-decarbonization release agent comprises the following steps:
s1 sepiolite powder 20 weight portions and Al2O315 parts by weight of Cr2O3Mixing 18 parts by weight of SiC21 parts by weight to obtain mixed powder;
s2 weighing 16 parts by weight of K2SiO3Adding the mixture into 45 parts by weight of water, stirring at 200rpm for 5min, and uniformly mixing to obtain a potassium silicate aqueous solution;
s3, adding the mixed powder obtained in the step S1 into the potassium silicate aqueous solution obtained in the step S2, and stirring by using an electric stirrer at the rotating speed of 600rpm for 15min to obtain a mixed coating;
s4, standing the mixed paint prepared in the step S3 at room temperature for 60min to obtain the decarburization-preventing parting agent.
Comparative example 2
The preparation method of the anti-decarbonization release agent comprises the following steps:
s1 Molai powder 30 weight portions, Al2O315 parts by weight of Cr2O3Mixing 18 parts by weight of SiC21 parts by weight to obtain mixed powder;
s2 weighing 16 parts by weight of K2SiO3Adding the mixture into 45 parts by weight of water, stirring at 200rpm for 5min, and uniformly mixing to obtain a potassium silicate aqueous solution;
s3, adding the mixed powder obtained in the step S1 into the potassium silicate aqueous solution obtained in the step S2, and stirring by using an electric stirrer at the rotating speed of 600rpm for 15min to obtain a mixed coating;
s4, standing the mixed paint prepared in the step S3 at room temperature for 60min to obtain the decarburization-preventing parting agent.
Example 2
The preparation method of the anti-decarbonization release agent comprises the following steps:
s1 weighing 30 parts by weight of mullite powder, 20 parts by weight of sepiolite powder and Al2O315 parts by weight of Cr2O318 parts by weight of SiC21 parts by weight, 1.5 parts by weight of wetting agent and 5 parts by weight of 1-butoxy-2-propanol are mixed uniformly to obtain mixed powder;
s2 weighing 16 parts by weight of K2SiO3Adding the mixture into 45 parts by weight of water, stirring at 200rpm for 5min, and uniformly mixing to obtain a potassium silicate aqueous solution;
s3, adding the mixed powder obtained in the step S1 into the potassium silicate aqueous solution obtained in the step S2, and stirring by using an electric stirrer at the rotating speed of 600rpm for 15min to obtain a mixed coating;
s4, standing the mixed paint prepared in the step S3 at room temperature for 60min to obtain the decarburization-preventing parting agent.
The wetting agent is prepared by adopting the following method: adding 8.5 parts by weight of methyl 2,2, 2-trifluoromethyl acrylate and 6.18 parts by weight of methylpropenyloxyethyltrimethyl ammonium chloride into 20mL of water, adding 3.4 parts by weight of diethylene glycol divinyl ether serving as a crosslinking agent, starting nitrogen protection, heating to 65 ℃, adding 0.05 part by weight of 2,2' -azobisisobutylamidine dihydrochloride serving as an initiator, heating to 80 ℃, and stirring for 4 hours to obtain the wetting agent.
The inventors found that the release agent mainly prepared from mullite powder and sepiolite powder has a problem of poor wettability between particles and fluid, and as the particulate matter increases, the dispersibility and stability of the release agent gradually decrease. Therefore, the invention adopts the polymerization reaction of the 2,2, 2-trifluoromethyl methacrylate and the methacryloxyethylene trimethyl ammonium chloride to prepare the wetting agent, the wetting agent can be adsorbed on the sepiolite powder and the mullite powder, the free energy of the sepiolite powder and the mullite powder is reduced, the roughness is increased, the dispersity and the stability of the separant are improved, the viscosity of the separant coating can be further reduced after the wetting agent is compounded with the 1-butoxy-2-propanol, and particularly, the separant is easy to peel after being heated and cooled at high temperature.
Example 3
The preparation method of the anti-decarbonization release agent comprises the following steps:
s1 weighing 30 parts by weight of mullite powder, 20 parts by weight of sepiolite powder and Al2O315 parts by weight of Cr2O3Mixing 18 parts by weight of SiC21 parts by weight of wetting agent 1.5 parts by weight to obtain mixed powder;
s2 weighing 16 parts by weight of K2SiO3Adding the mixture into 45 parts by weight of water, stirring at 200rpm for 5min, and uniformly mixing to obtain a potassium silicate aqueous solution;
s3, adding the mixed powder obtained in the step S1 into the potassium silicate aqueous solution obtained in the step S2, and stirring by using an electric stirrer at the rotating speed of 600rpm for 15min to obtain a mixed coating;
s4, standing the mixed paint prepared in the step S3 at room temperature for 60min to obtain the decarburization-preventing parting agent.
The wetting agent is prepared by adopting the following method: adding 8.5 parts by weight of methyl 2,2, 2-trifluoromethyl acrylate and 6.18 parts by weight of methylpropenyloxyethyltrimethyl ammonium chloride into 20mL of water, adding 3.4 parts by weight of diethylene glycol divinyl ether serving as a crosslinking agent, starting nitrogen protection, heating to 65 ℃, adding 0.05 part by weight of 2,2' -azobisisobutylamidine dihydrochloride serving as an initiator, heating to 80 ℃, and stirring for 4 hours to obtain the wetting agent.
Example 4
The preparation method of the anti-decarbonization release agent comprises the following steps:
s1 weighing 30 parts by weight of mullite powder, 20 parts by weight of sepiolite powder and Al2O315 parts by weight of Cr2O3Mixing 18 parts by weight of SiC21 parts by weight and 5 parts by weight of 1-butoxy-2-propanol uniformly to obtain mixed powder;
s2 weighing 16 parts by weight of K2SiO3Adding the mixture into 45 parts by weight of water, stirring at 200rpm for 5min, and uniformly mixing to obtain a potassium silicate aqueous solution;
s3, adding the mixed powder obtained in the step S1 into the potassium silicate aqueous solution obtained in the step S2, and stirring by using an electric stirrer at the rotating speed of 600rpm for 15min to obtain a mixed coating;
s4, standing the mixed paint prepared in the step S3 at room temperature for 60min to obtain the decarburization-preventing parting agent.
Test example 1
The adopted sample base material is spring steel 1070, the surface of the sample is cleaned, the decarburization-preventing isolating agent obtained in examples 1-4 and comparative examples 1 and 2 is coated on the surface of the sample and then naturally dried, and 3 parallel samples are arranged in blank groups for testing without using an isolating agent. According to the requirements of heat treatment conditions of parts, placing a sample into a 600 ℃ heating furnace, preserving heat for 1h, discharging, air cooling to room temperature, moving to 1250 ℃, preserving heat for 3h, performing oil quenching, and observing the macro morphology of the sample. A sample is corroded by 4% nitric acid alcohol according to a decarburized layer depth determination method of GB/T224-2019 steel, the decarburized layer depth is measured from the edge of the sample to a position where the hardness value is stable in one microscopic view field of the deepest uniform decarburizing area by using a Vickers microhardness tester, the average value of 3 times of measurement is taken as the decarburized layer depth, and the test result is shown in table 1.
TABLE 1 decarbonization preventing Effect test
Thickness of decarburized layer (mm)
Example 1 0.40
Example 2 0.28
Example 3 0.41
Example 4 0.39
Comparative example 1 0.64
Comparative example 2 0.52
Blank group 1.15
As can be seen from Table 1, the decarbonization preventing performance of the separant can be effectively improved by compounding sepiolite powder and mullite powder and adding the sepiolite powder and the mullite powder into the preparation of the decarbonization preventing separant, and substances such as silicon carbide powder and the like firstly react with oxygen at a low temperature stage, so that the oxygen potential near a coating is reduced, and a substrate is protected from being oxidized; as the temperature rises, high-melting point oxides such as alumina, silicon carbide and mullite powder are used as frameworks, and the suspension formed by the sepiolite powder enables framework substances to form a disordered fiber network in trapped liquid, so that the contact between a heating atmosphere and a matrix is isolated, the protection effect in a high-temperature stage is achieved, and the protection coating plays a protection effect in a wider temperature range. In addition, as can be seen from comparison of examples 2 to 4, the decarbonization preventing performance of the isolating agent can be further enhanced by adding the wetting agent, and the wetting agent prepared by the method can be effectively adsorbed on sepiolite powder and mullite powder, so that the free energy of the sepiolite powder and the mullite powder is reduced, the roughness is increased, the combination of the sepiolite powder and the mullite powder with the fluid time is tighter, and the protective layer effect of the isolating agent is enhanced.
Test example 2
The adopted sample base material is spring steel 1070, the surface of the sample is cleaned, the anti-decarbonization isolating agent obtained in examples 1-4 and comparative examples 1 and 2 is coated on the surface of the sample, the sample is naturally dried, and 3 parallel samples are arranged for testing. And (3) putting the sample into a 600 ℃ heating furnace, preserving heat for 1h, discharging, cooling to room temperature, moving to 1250 ℃ for preserving heat for 1h, performing oil quenching, cooling by using 20# engine oil after oil quenching, and detecting the falling area of the coating, wherein the test result is shown in table 2.
TABLE 2 Release agent Release Rate
The ratio of the area of falling off%
Example 1 85
Example 2 98
Example 3 91
Example 4 92
Comparative example 1 80
Comparative example 2 82
When the coating is in a low-temperature stage, silicon carbide and oxygen react to generate silicon oxide, so that the oxygen potential is reduced; SiO 22Reacting with ferric oxide on the surface of the steel part at high temperature to generate a ceramic layer (fayalite) which is easy to peel off; a12O3The chemical stability is high, and the heat resistance of the coating can be improved; the sepiolite powder and the mullite powder can increase the melting temperature of the glass enamel and make the coating inert to certain steel, and the further introduction of the wetting agent and the 1-butoxy-2-propanol can obviously improve the shedding property of the separant, and can be related to the effect that the wetting agent and the 1-butoxy-2-propanol are compounded to act between colloidal particles and a separant matrix to well reduce the viscosity. Especially, after high-temperature heating and cooling, the release agent coating on the surface of the workpiece can be automatically peeled off, so that the post-treatment cost is saved.
The foregoing detailed description of the preferred embodiments of the invention has been presented. It should be understood that numerous modifications and variations could be devised by those skilled in the art in light of the present teachings without departing from the inventive concepts. Therefore, the technical solutions available to those skilled in the art through logic analysis, reasoning and limited experiments based on the prior art according to the concept of the present invention should be within the scope of protection defined by the claims.

Claims (6)

1. The anti-decarbonization release agent is characterized by comprising the following raw materials: mineral powder, Al2O3、Cr2O3SiC, binder and water.
2. The anti-decarbonization release agent is characterized by comprising the following raw materials: mullite powder, sepiolite powder, Al2O3、Cr2O3SiC, binder and water.
3. An anti-decarbonization separant is characterized in that,the feed comprises the following raw materials in parts by weight: 10-38 parts of mullite powder, 10-20 parts of sepiolite powder and Al2O310 to 25 parts of Cr2O310-25 parts of SiC, 10-25 parts of a binder, 8-20 parts of a binder and 30-50 parts of water.
4. The anti-decarbonization release agent as claimed in claim 1, 2 or 3, wherein: the binder is K2SiO3
5. The anti-decarbonization release agent as claimed in claim 1, 2 or 3, wherein: the Al is2O3、Cr2O3The SiC is fine powder, the purity is more than 99%, and the particle sizes are respectively 500-1000 meshes independently.
6. The method for preparing the anti-decarbonization release agent according to any one of claims 1 to 5, which comprises the following steps:
s1 weighing the raw materials according to the formula, mixing mullite powder, sepiolite powder and Al2O3、Cr2O3Mixing SiC evenly to obtain mixed powder;
s2 reaction of K2SiO3Mixing with water, and stirring at 200-300 rpm for 5-10 min to obtain potassium silicate aqueous solution;
s3, adding the mixed powder obtained in the step S1 into the potassium silicate aqueous solution obtained in the step S2, and stirring at the rotating speed of 500-600 rpm for 15-20 min to obtain a mixed coating;
s4, standing the mixed coating prepared in the step S3 at room temperature for 30-60 min to obtain the decarburization isolating agent.
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