Magnesium aluminate spinel enhanced magnesia-based foamed ceramic filter and preparation method thereof

A magnesia-aluminum spinel, foam ceramic technology, applied in magnesia-aluminum spinel reinforced magnesia-based foam ceramic filter and its preparation, filtration and purification of aluminum and its alloy melt, magnesia-based foam ceramic filter and In the field of its preparation, it can solve the problems of increasing matrix magnesium oxide lattice distortion, operation limitation, myocardial toxicity, etc., and achieve the effects of excellent chemical stability, good strength and simple process.

Active Publication Date: 2018-09-11
NANJING UNIV OF AERONAUTICS & ASTRONAUTICS
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Problems solved by technology

Chinese patent documents CN1011306B (pure magnesia foam ceramic filter and its preparation process), CN101138691A (preparation method of magnesia foam ceramic filter for casting), etc., prepare foam ceramics with pure magnesia as raw material, because MgO has a very high melting point and coefficient of thermal expansion (13.5×10 -6 / °C) is high, therefore, it leads to difficult sintering (sintering temperature is not lower than 0.8 times its melting point) and poor thermal shock resistance, which limits the application and development of MgO foam ceramics
add V 2 o 5 In powder form, MgO will react with V at 1190°C 2 o 5 form an approximate composition of Mg 3 V 2 o 8 The liquid phase promotes sintering and can significantly reduce the sintering temperature of MgO foam ceramics, but V 2 o 5 Harmful to the respiratory system and skin during use, and has strict restrictions on operation
with V 2 o 5 Similarly, cobalt oxide is also a good low-temperature sintering aid, but its application is limited as a highly toxic substance and rare resource
Fluoride is a strong co-solvent and mineralizer commonly used in ceramic industry sintering, Chinese patent documents CN100536986C (magnesia foam ceramic filter), CN1473947A (foam ceramic for magnesium and magnesium alloy melt purification), CN101785944B (for magnesium Fluorite (melting point 1423°C) and magnesium fluoride (melting point 1248°C) are added to the preparation method of magnesium oxide foam ceramic filter for magnesium melt filtration. The solid solution of fluoride not only increases the oxidation of the matrix during the sintering process The lattice of magnesium is distorted, and it is easy to form a low-melting liquid phase, thereby reducing the sintering temperature of magnesia ceramics; however, during the sintering process, F in fluoride combines with Si, Al, Fe, and Ca, and most (in ceramic tiles) About 70% in production) volatilization in gaseous form not only erodes the green body itself and damages the quality of sintered ceramics, but more seriously, it will cause fluoride pollution when discharged into the atmosphere. Fluoride can enter the human body through the respiratory tract, digestive tract and skin , has a toxic effect on the central nervous system and myocardium, and low-concentration fluorine pollution can lead to brittle calcification of teeth and bones. The discharge standard of fluoride must be lower than 5.0mg / m2 in the "Ceramic Industry Pollutant Discharge Standard" (GB25464-2010) 3 Therefore, using fluoride as a low-temperature sintering aid for magnesia ceramics will inevitably increase the emission of gaseous fluoride and increase the burden of environmental protection investment; in addition, fluoride ions in the residual solid-solution fluoride in ceramics exist in the form of replacing oxygen ions, resulting in crystal The chemical stability of the intergranular bonding is reduced, and it is difficult to resist the long-term erosion of flux inclusions in the magnesium melt
Water glass, silica sol and ethyl silicate are used as binders in the preparation slurry of the disclosed ceramic foam filters such as Chinese patent literature CN101138691A, and the SiO between the sintered ceramic foam particles 2 The presence of components makes it easy to react with magnesium and its alloy melts according to (4), which also reduces the chemical stability of foamed ceramics
However, diboron trioxide is easy to react with magnesium and aluminum, and is not stable in magnesium and aluminum alloy melts; at the same time, because diboron trioxide is soluble in solvents such as water and ethanol, it can strongly absorb water in the air to form boric acid. The diboron trioxide added in the preparation process of foam ceramics is dissolved in water to form a boric acid aqueous solution, which is easy to react with magnesium oxide to form magnesium borate precipitation and reduce its effect
Gallium oxide is a homogeneous oxide of diboron trioxide, which forms spinel-type MgGa with magnesium oxide at a lower temperature 2 o 4 It plays a role in reducing the sintering temperature, but the amount of gallium resources is very small (gallium is a strategic reserve metal), and the high price of gallium oxide limits its application in ordinary ceramics.

Method used

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  • Magnesium aluminate spinel enhanced magnesia-based foamed ceramic filter and preparation method thereof
  • Magnesium aluminate spinel enhanced magnesia-based foamed ceramic filter and preparation method thereof
  • Magnesium aluminate spinel enhanced magnesia-based foamed ceramic filter and preparation method thereof

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Effect test

Embodiment 1

[0050] According to the proportion that nano-alumina accounts for 4% of the mass of ceramic powder, weigh nano-γ-Al with a particle size of 30nm 2 o 3 The powder and particle size are 250 mesh (diameter d 50 Prepare ceramic powder for 58 μm) fused magnesia powder; mix and prepare rheological agent according to the mass ratio of polyvinyl alcohol and methyl cellulose at a ratio of 2:3.

[0051] According to mass percentage, 10% of nano-alumina sol with a solid content of 20% (select a commercial nano-alumina sol with a near-neutral pH value, the same below), 0.8% of rheological agent, and the rest are ceramic powders for batching. First, add magnesium oxide powder into the ball mill tank according to the proportion, prepare nano-aluminum sol, rheological agent and appropriate amount of deionized water (the amount to be added is determined according to the solid content of the ceramic slurry, the same below) to prepare a solution, and then add nano- γ-Al 2 o 3 Powder, sonica...

Embodiment 2

[0055] According to the proportion that nano-alumina accounts for 8% of the mass of ceramic powder, weigh nano-γ-Al with a particle size of 60nm 2 o 3 The powder and particle size are 500 mesh (diameter d 50 Prepare ceramic powder for fused magnesia powder (25 μm); mix and prepare rheological agent according to the mass ratio of polyvinyl alcohol and hydroxypropyl methylcellulose at a ratio of 2:3.

[0056] According to mass percentage, 15% of nano-alumina sol with a solid content of 25%, 1.5% of rheological agent, and the rest are ceramic powder for batching. First, add magnesium oxide powder into the ball mill tank according to the proportion, prepare nano-aluminum sol, rheological agent and appropriate amount of deionized water into a solution, and then add nano-γ-Al 2 o 3 Powder, sonicated for 45 minutes to make nanometer γ-Al 2 o 3After the powder is fully dispersed in the solution, add it to the ball mill tank, then add corundum balls according to the ratio of ball ...

Embodiment 3

[0060] According to the ratio that nano-alumina accounts for 6% of the mass of ceramic powder, weigh nano-γ-Al with a particle size of 50nm 2 o 3 The powder and particle size are 325 mesh (diameter d 50 Prepare ceramic powder for fused magnesia powder (45 μm); mix and prepare rheological agent according to the mass ratio of polyvinyl alcohol and hydroxyethyl cellulose at a ratio of 2:3.

[0061] According to mass percentage, 20% of nano-alumina sol with a solid content of 22%, 1.0% of rheological agent, and the rest are ceramic powder for batching. First, add magnesium oxide powder into the ball mill tank according to the proportion, prepare nano-aluminum sol, rheological agent and appropriate amount of deionized water into a solution, and then add nano-γ-Al 2 o 3 Powder, sonicated for 60 minutes to make nanometer γ-Al 2 o 3 After the powder is fully dispersed in the solution, add it to the ball mill tank, and then add corundum balls according to the ratio of ball to mate...

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Abstract

The invention discloses a magnesium aluminate spinel enhanced magnesia-based foamed ceramic filter with capability of realizing sintering at low temperature, excellent chemical stability and excellentthermal shock resistant performance, and a preparation method thereof. The preparation method comprises the following steps that (1) 10 to 20 percent of nanometer alumina sol, 0.8 to 1.5 percent of rheological agents and the balance of magnesium oxide ceramic powder containing a nanometer aluminum oxide sintering aid are proportioned; deionized water is added; ball milling and uniform mixing areperformed; then, through vacuum exhaust, ceramic slurry with the solid content being 60 to 70 percent is prepared; (2) a polyurethane foamed plastic template is soaked into the ceramic slurry; the polyurethane foamed plastic template is extruded through a roller press for removing the redundant leaching hanging slurry; then, biscuit is prepared; then, the biscuit is heated to 80 to 120 DEG C for drying; (3) the dried biscuit is put into a sintering furnace; the temperature is raised to 1400 to 1600 DEG C; high-temperature sintering is performed; cooling is performed along with the furnace to room temperature; the magnesia-based foamed ceramic filter is obtained.

Description

technical field [0001] The invention relates to a magnesium oxide-based foam ceramic filter and a preparation method thereof, in particular to a magnesium-aluminum spinel reinforced magnesium oxide-based foam ceramic filter and a preparation method thereof, belonging to the field of metal materials and metallurgy. The filter prepared by the invention is particularly suitable for filtering and purifying magnesium and its alloy melts, and can also be used for filtering and purifying aluminum and its alloy melts. Background technique [0002] Magnesium is chemically active. During casting and processing, it is very easy to chemically react with oxygen, nitrogen and water vapor. The resulting products remain in the magnesium, affecting the internal quality of the product and deteriorating the performance of the product. According to the types and properties of inclusions in magnesium alloys, inclusions are generally divided into two categories: metal inclusions and non-metal inc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/053C04B35/63C04B35/634C04B35/636C04B35/64C04B38/06B01D39/20
CPCB01D39/2093C04B35/053C04B35/6303C04B35/63416C04B35/6365C04B35/64C04B38/0615C04B2235/3218C04B2235/322C04B2235/3222C04B2235/5436C04B2235/5454C04B2235/6562C04B2235/6567
Inventor 刘子利刘希琴刘思雨
Owner NANJING UNIV OF AERONAUTICS & ASTRONAUTICS
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