CN114380606A - Preparation process of machined high-strength refractory material - Google Patents
Preparation process of machined high-strength refractory material Download PDFInfo
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- CN114380606A CN114380606A CN202210003770.6A CN202210003770A CN114380606A CN 114380606 A CN114380606 A CN 114380606A CN 202210003770 A CN202210003770 A CN 202210003770A CN 114380606 A CN114380606 A CN 114380606A
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- 239000011819 refractory material Substances 0.000 title claims abstract description 69
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000000463 material Substances 0.000 claims abstract description 109
- 239000000843 powder Substances 0.000 claims abstract description 59
- 238000002156 mixing Methods 0.000 claims abstract description 49
- 238000000227 grinding Methods 0.000 claims abstract description 47
- 238000000498 ball milling Methods 0.000 claims abstract description 42
- 238000005245 sintering Methods 0.000 claims abstract description 36
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 26
- 238000001816 cooling Methods 0.000 claims abstract description 26
- 238000000034 method Methods 0.000 claims abstract description 25
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000001035 drying Methods 0.000 claims abstract description 21
- 238000005507 spraying Methods 0.000 claims abstract description 21
- 239000007864 aqueous solution Substances 0.000 claims abstract description 13
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 13
- 238000003825 pressing Methods 0.000 claims abstract description 11
- 238000005303 weighing Methods 0.000 claims abstract description 11
- 238000010438 heat treatment Methods 0.000 claims description 74
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical class O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 45
- 239000002994 raw material Substances 0.000 claims description 37
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims description 32
- 239000000292 calcium oxide Substances 0.000 claims description 32
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 32
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 24
- 239000000835 fiber Substances 0.000 claims description 24
- 229910052814 silicon oxide Inorganic materials 0.000 claims description 22
- 238000001354 calcination Methods 0.000 claims description 20
- 238000000465 moulding Methods 0.000 claims description 20
- 239000002245 particle Substances 0.000 claims description 20
- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 claims description 20
- 229910001948 sodium oxide Inorganic materials 0.000 claims description 20
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 19
- WGLPBDUCMAPZCE-UHFFFAOYSA-N Trioxochromium Chemical compound O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 claims description 13
- 239000000126 substance Substances 0.000 claims description 13
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 12
- 230000005294 ferromagnetic effect Effects 0.000 claims description 12
- 239000000395 magnesium oxide Substances 0.000 claims description 12
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 12
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 12
- 238000007885 magnetic separation Methods 0.000 claims description 12
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 claims description 12
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 12
- 229910000423 chromium oxide Inorganic materials 0.000 claims description 11
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Inorganic materials O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 claims description 11
- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 claims description 11
- 238000004140 cleaning Methods 0.000 claims description 10
- 239000011812 mixed powder Substances 0.000 claims description 10
- 238000004519 manufacturing process Methods 0.000 claims description 7
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 6
- 239000003245 coal Substances 0.000 claims description 2
- 239000000377 silicon dioxide Substances 0.000 claims 1
- 239000002817 coal dust Substances 0.000 description 8
- 238000009776 industrial production Methods 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000005336 cracking Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000007769 metal material Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008602 contraction Effects 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000003779 heat-resistant material Substances 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 150000002843 nonmetals Chemical class 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
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Abstract
The invention discloses a preparation process of a machined high-strength refractory material, which belongs to the technical field of refractory materials and comprises the steps of weighing raw and auxiliary materials according to mass percentage, crushing, mixing, grinding and presintering the raw and auxiliary materials to obtain material powder, ball-milling and mixing the material powder in absolute ethyl alcohol which is several times of the weight of the material powder for a plurality of hours, drying the material powder after ball-milling and mixing, dry-pressing and forming the material powder under strong pressure, uniformly spraying a sodium carbonate aqueous solution in the forming process to finally obtain a refractory material green body, sintering the formed refractory material green body for a plurality of hours at high temperature, and naturally cooling to room temperature after sintering to obtain the refractory material.
Description
Technical Field
The invention belongs to the technical field of refractory materials, and particularly relates to a preparation process of a machined high-strength refractory material.
Background
The modern metallurgy and other related industries need the high-temperature structure refractory material to have excellent comprehensive performance, wherein the mechanical property, thermal shock resistance, oxidation resistance and machinability are most important, and in the traditional sense, the refractory material is an inorganic non-metallic material with the refractoriness of not less than 1580 ℃, is a basic material serving for high-temperature technology, is a structural material used for thermal equipment such as a high-temperature kiln and the like, and a material for industrial high-temperature containers and parts, and can bear corresponding physical and chemical changes and mechanical actions.
The poor mechanical toughness of inorganic non-metallic materials is the problem of poor mechanical toughness commonly existing in inorganic non-metals and materials, and particularly under the condition that the integrity of the refractory material is affected by cracking, peeling and the like of the refractory material under the action of expansion with heat and contraction with cold due to the fact that gaps between rapid cooling and rapid heating and used gaps are large in temperature difference, the service life of the refractory material is shortened.
Disclosure of Invention
Aiming at the problem that cracks are easy to generate in the existing rapid cooling and heating environment, the invention provides a preparation process of a machining high-strength refractory material.
In order to solve the problems, the invention adopts the following technical scheme:
a preparation process of a machined high-strength refractory material is characterized by comprising the following steps:
step 1, weighing each raw and auxiliary material according to the mass percentage, crushing, mixing, grinding and presintering the raw and auxiliary materials to obtain material powder;
step 2, ball-milling and mixing the material powder treated in the step 1 in absolute ethyl alcohol of which the weight is 2-3 times that of the material powder for 3-5 hours, and drying the material powder after ball-milling and mixing;
step 3, dry-pressing and molding the material powder treated in the step 2 under the pressure of 100-150 MPa, and uniformly spraying 0.05-0.1 mol/L sodium carbonate aqueous solution with the mass of 6-10% of the raw material in the molding process to finally prepare a refractory material green body;
and 4, sintering the molded refractory material green body at 1200-1400 ℃ for 3-5 hours, roasting at 2200-2400 ℃ for 10 hours, and naturally cooling to room temperature to obtain the refractory material.
Preferably, the mass percentages of the raw materials and the auxiliary materials in the step 1 are as follows:
30-50% of aluminum oxide;
20-30% of chromium oxide;
15-40% of silicon oxide;
5-10% of calcium oxide;
3-5% of magnesium oxide;
1-2% of titanium oxide;
1-2% of yttrium oxide;
0.5-1% of niobium pentoxide;
10-15% of modified zirconia fiber.
In order to increase the binding property between the zirconia fiber and the raw and auxiliary materials, further, the modified zirconia fiber is prepared by the following steps: 50 parts of zirconia, 3 parts of calcium oxide and 1 part of sodium oxide are added, and the molar ratio of 400 parts of calcium oxide to 400 parts of sodium oxide is 1: 1, grinding for 10-15 hours by taking absolute ethyl alcohol as a grinding medium, calcining for 5-8 hours at 800-1000 ℃, grinding, cleaning and drying after calcining and cooling.
In order to increase the contact area between the silicon oxide and other raw materials and ensure more sufficient reaction, the silicon oxide has a particle size of 200-500 nm and a purity of 95 wt%.
In order to increase the contact area between the alumina and other raw materials and ensure more sufficient reaction, the particle size of the alumina is 100-500 nm, and the purity of the alumina is 98 wt%.
In order to remove other impurities and prevent the impurities from affecting the quality of the refractory material, preferably, the raw and auxiliary materials are crushed in the step 1 and then subjected to magnetic separation treatment to remove ferromagnetic substances therein.
In order to prevent the insufficient stability of the heat-resistant material caused by direct high-temperature heating, preferably, the raw material mixing, grinding and pre-sintering in the step 1 comprises the following specific steps: mixing and grinding the raw materials, mixing the raw materials with coal powder accounting for 6-8 wt% of the weight of the raw materials, uniformly mixing and grinding, spraying the mixed powder into a rotary kiln for sintering, heating to 180-230 ℃, preserving heat for 1-1.5 hours, heating to 550-600 ℃, preserving heat for 0.5-1 hour, heating to 900-1000 ℃, sintering for 2-3 hours, and continuously rotating the rotary kiln in the sintering process.
In order to ensure that the raw and auxiliary materials in the rotary kiln can be fully reacted by gradually heating, the heating rate in the rotary kiln is 3-5 ℃/min.
In order to enable the material powder to fully react with the absolute ethyl alcohol, the ball milling rotation speed during ball milling in the step 2 is preferably 1800-2300 rpm.
In order to prevent cracking of the refractory green body caused by too fast temperature rise, the temperature rise rate in the step 4 is preferably 5-10 ℃/min.
Compared with the prior art, the invention provides a preparation process of a machined high-strength refractory material, which has the following beneficial effects:
the invention adjusts the formula of the refractory material, adjusts the mass percentage of each raw and auxiliary material in the formula, improves the content of alumina and chromic oxide, improves the use strength of the material, changes the manufacturing method according to the adjusted formula, crushes the raw and auxiliary materials according to the adding sequence, grinds and stirs the raw and auxiliary materials, adds magnetic separation treatment, can remove ferromagnetic substances, improves the purity of the material, finally uses a step-by-step heating mode to gradually heat in the heating process, improves the hardness of the refractory material, wherein the modified zirconia fiber is taken as a toughness material to be tightly combined with the products of alumina, chromic oxide, silicon oxide, calcium oxide, magnesium oxide and titanium oxide converted at high temperature, and simultaneously utilizes yttrium oxide to keep the stability and corrosion resistance of the modified zirconia fiber, the refractory material has extremely high toughness, can not generate a large amount of cracks in a rapid cooling and heating use environment, has long service life, and can better meet the requirements of industrial production.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments.
Example 1:
a preparation process of a machined high-strength refractory material comprises the following steps:
step 1, weighing raw and auxiliary materials according to mass percentage, wherein 30% of aluminum oxide, 20% of chromium oxide, 25% of silicon oxide, 9% of calcium oxide, 3% of magnesium oxide, 1% of titanium oxide, 1% of yttrium oxide, 1% of niobium pentoxide and 10% of modified zirconia fiber, crushing the raw and auxiliary materials, carrying out magnetic separation treatment to remove ferromagnetic substances in the raw and auxiliary materials, then mixing the mixed raw materials with coal dust accounting for 8 wt% of the raw materials, uniformly mixing and grinding, spraying the mixed powder into a rotary kiln to sinter, heating to 230 ℃, keeping the temperature for 1.5 hours, heating to 600 ℃, keeping the temperature for 1 hour, heating to 1000 ℃, sintering for 3 hours, continuously rotating the rotary kiln in the sintering process, and obtaining material powder when the heating rate in the rotary kiln is 5 ℃/min;
wherein the particle size of the silicon oxide is 500nm, the purity is 95 wt%, the particle size of the aluminum oxide is 500nm, the purity is 98 wt%, and the modified zirconia fiber is prepared by the following steps: 50 parts of zirconia, 3 parts of calcium oxide and 1 part of sodium oxide are added, and the molar ratio of 400 parts of calcium oxide to 400 parts of sodium oxide is 1: 1, grinding for 15 hours by using absolute ethyl alcohol as grinding medium, calcining for 8 hours at the temperature of 1000 ℃, grinding, cleaning and drying after calcining and cooling
Step 2, ball-milling and mixing the material powder treated in the step 1 in absolute ethyl alcohol of which the weight is 3 times that of the material powder for 5 hours, wherein the ball-milling rotating speed during ball-milling is 2300rpm, and drying the material powder after ball-milling and mixing;
step 3, dry-pressing and molding the material powder treated in the step 2 under the pressure of 150MPa, and uniformly spraying 0.1mol/L sodium carbonate aqueous solution with the mass of 10% of the raw materials in the molding process to finally prepare a refractory material green body;
and 4, sintering the molded refractory material green body at 1400 ℃ for 5 hours, roasting at 2400 ℃ and keeping the temperature for 10 hours, wherein the heating rate during heating is 10 ℃/min, and naturally cooling to room temperature after the heating is finished to obtain the refractory material.
Example 2:
a preparation process of a machined high-strength refractory material comprises the following steps:
step 1, weighing raw and auxiliary materials according to mass percentage, wherein 35% of aluminum oxide, 20% of chromium oxide, 20% of silicon oxide, 9% of calcium oxide, 3% of magnesium oxide, 1% of titanium oxide, 1% of yttrium oxide, 1% of niobium pentoxide and 10% of modified zirconia fiber, crushing the raw and auxiliary materials, carrying out magnetic separation treatment to remove ferromagnetic substances in the raw and auxiliary materials, then mixing the mixed raw materials with coal dust accounting for 8 wt% of the raw materials, uniformly mixing and grinding, spraying the mixed powder into a rotary kiln to sinter, heating to 230 ℃, keeping the temperature for 1.5 hours, heating to 600 ℃, keeping the temperature for 1 hour, heating to 1000 ℃, sintering for 3 hours, continuously rotating the rotary kiln in the sintering process, and obtaining material powder when the heating rate in the rotary kiln is 5 ℃/min;
wherein the particle size of the silicon oxide is 500nm, the purity is 95 wt%, the particle size of the aluminum oxide is 500nm, the purity is 98 wt%, and the modified zirconia fiber is prepared by the following steps: 50 parts of zirconia, 3 parts of calcium oxide and 1 part of sodium oxide are added, and the molar ratio of 400 parts of calcium oxide to 400 parts of sodium oxide is 1: 1, grinding for 15 hours by using absolute ethyl alcohol as grinding medium, calcining for 8 hours at the temperature of 1000 ℃, grinding, cleaning and drying after calcining and cooling
Step 2, ball-milling and mixing the material powder treated in the step 1 in absolute ethyl alcohol of which the weight is 3 times that of the material powder for 5 hours, wherein the ball-milling rotating speed during ball-milling is 2300rpm, and drying the material powder after ball-milling and mixing;
step 3, dry-pressing and molding the material powder treated in the step 2 under the pressure of 150MPa, and uniformly spraying 0.1mol/L sodium carbonate aqueous solution with the mass of 10% of the raw materials in the molding process to finally prepare a refractory material green body;
and 4, sintering the molded refractory material green body at 1400 ℃ for 5 hours, roasting at 2400 ℃ and keeping the temperature for 10 hours, wherein the heating rate during heating is 10 ℃/min, and naturally cooling to room temperature after the heating is finished to obtain the refractory material.
Example 3:
a preparation process of a machined high-strength refractory material comprises the following steps:
step 1, weighing raw and auxiliary materials according to mass percentage, wherein 35% of aluminum oxide, 20% of chromium oxide, 24% of silicon oxide, 5% of calcium oxide, 3% of magnesium oxide, 1% of titanium oxide, 1% of yttrium oxide, 1% of niobium pentoxide and 10% of modified zirconia fiber, crushing the raw and auxiliary materials, carrying out magnetic separation treatment to remove ferromagnetic substances in the raw and auxiliary materials, then mixing the mixed raw materials with coal dust accounting for 8 wt% of the raw materials, uniformly mixing and grinding, spraying the mixed powder into a rotary kiln to sinter, heating to 230 ℃, keeping the temperature for 1.5 hours, heating to 600 ℃, keeping the temperature for 1 hour, heating to 1000 ℃, sintering for 3 hours, continuously rotating the rotary kiln in the sintering process, and obtaining material powder when the heating rate in the rotary kiln is 5 ℃/min;
wherein the particle size of the silicon oxide is 500nm, the purity is 95 wt%, the particle size of the aluminum oxide is 500nm, the purity is 98 wt%, and the modified zirconia fiber is prepared by the following steps: 50 parts of zirconia, 3 parts of calcium oxide and 1 part of sodium oxide are added, and the molar ratio of 400 parts of calcium oxide to 400 parts of sodium oxide is 1: 1, grinding for 15 hours by using absolute ethyl alcohol as grinding medium, calcining for 8 hours at the temperature of 1000 ℃, grinding, cleaning and drying after calcining and cooling
Step 2, ball-milling and mixing the material powder treated in the step 1 in absolute ethyl alcohol of which the weight is 3 times that of the material powder for 5 hours, wherein the ball-milling rotating speed during ball-milling is 2300rpm, and drying the material powder after ball-milling and mixing;
step 3, dry-pressing and molding the material powder treated in the step 2 under the pressure of 150MPa, and uniformly spraying 0.1mol/L sodium carbonate aqueous solution with the mass of 10% of the raw materials in the molding process to finally prepare a refractory material green body;
and 4, sintering the molded refractory material green body at 1400 ℃ for 5 hours, roasting at 2400 ℃ and keeping the temperature for 10 hours, wherein the heating rate during heating is 10 ℃/min, and naturally cooling to room temperature after the heating is finished to obtain the refractory material.
Example 4:
a preparation process of a machined high-strength refractory material comprises the following steps:
step 1, weighing raw and auxiliary materials according to mass percentage, wherein 33% of aluminum oxide, 22% of chromium oxide, 24% of silicon oxide, 5% of calcium oxide, 3% of magnesium oxide, 1% of titanium oxide, 1% of yttrium oxide, 1% of niobium pentoxide and 10% of modified zirconia fiber, crushing the raw and auxiliary materials, carrying out magnetic separation treatment to remove ferromagnetic substances in the raw and auxiliary materials, then mixing the mixed raw materials with coal dust accounting for 8 wt% of the raw materials, uniformly mixing and grinding, spraying the mixed powder into a rotary kiln to sinter, heating to 230 ℃, keeping the temperature for 1.5 hours, heating to 600 ℃, keeping the temperature for 1 hour, heating to 1000 ℃, sintering for 3 hours, continuously rotating the rotary kiln in the sintering process, and obtaining material powder when the heating rate in the rotary kiln is 5 ℃/min;
wherein the particle size of the silicon oxide is 500nm, the purity is 95 wt%, the particle size of the aluminum oxide is 500nm, the purity is 98 wt%, and the modified zirconia fiber is prepared by the following steps: 50 parts of zirconia, 3 parts of calcium oxide and 1 part of sodium oxide are added, and the molar ratio of 400 parts of calcium oxide to 400 parts of sodium oxide is 1: 1, grinding for 15 hours by using absolute ethyl alcohol as grinding medium, calcining for 8 hours at the temperature of 1000 ℃, grinding, cleaning and drying after calcining and cooling
Step 2, ball-milling and mixing the material powder treated in the step 1 in absolute ethyl alcohol of which the weight is 3 times that of the material powder for 5 hours, wherein the ball-milling rotating speed during ball-milling is 2300rpm, and drying the material powder after ball-milling and mixing;
step 3, dry-pressing and molding the material powder treated in the step 2 under the pressure of 150MPa, and uniformly spraying 0.1mol/L sodium carbonate aqueous solution with the mass of 10% of the raw materials in the molding process to finally prepare a refractory material green body;
and 4, sintering the molded refractory material green body at 1400 ℃ for 5 hours, roasting at 2400 ℃ and keeping the temperature for 10 hours, wherein the heating rate during heating is 10 ℃/min, and naturally cooling to room temperature after the heating is finished to obtain the refractory material.
Example 5:
a preparation process of a machined high-strength refractory material comprises the following steps:
step 1, weighing raw and auxiliary materials according to mass percentage, wherein 39% of aluminum oxide, 22% of chromium oxide, 18% of silicon oxide, 5% of calcium oxide, 3% of magnesium oxide, 1% of titanium oxide, 1% of yttrium oxide, 1% of niobium pentoxide and 10% of modified zirconia fiber, crushing the raw and auxiliary materials, carrying out magnetic separation treatment to remove ferromagnetic substances in the raw and auxiliary materials, then mixing the mixed raw materials with coal dust accounting for 8 wt% of the raw materials, uniformly mixing and grinding, spraying the mixed powder into a rotary kiln to sinter, heating to 230 ℃, keeping the temperature for 1.5 hours, heating to 600 ℃, keeping the temperature for 1 hour, heating to 1000 ℃, sintering for 3 hours, continuously rotating the rotary kiln in the sintering process, and obtaining material powder when the heating rate in the rotary kiln is 5 ℃/min;
wherein the particle size of the silicon oxide is 500nm, the purity is 95 wt%, the particle size of the aluminum oxide is 500nm, the purity is 98 wt%, and the modified zirconia fiber is prepared by the following steps: 50 parts of zirconia, 3 parts of calcium oxide and 1 part of sodium oxide are added, and the molar ratio of 400 parts of calcium oxide to 400 parts of sodium oxide is 1: 1, grinding for 15 hours by using absolute ethyl alcohol as grinding medium, calcining for 8 hours at the temperature of 1000 ℃, grinding, cleaning and drying after calcining and cooling
Step 2, ball-milling and mixing the material powder treated in the step 1 in absolute ethyl alcohol of which the weight is 3 times that of the material powder for 5 hours, wherein the ball-milling rotating speed during ball-milling is 2300rpm, and drying the material powder after ball-milling and mixing;
step 3, dry-pressing and molding the material powder treated in the step 2 under the pressure of 150MPa, and uniformly spraying 0.1mol/L sodium carbonate aqueous solution with the mass of 10% of the raw materials in the molding process to finally prepare a refractory material green body;
and 4, sintering the molded refractory material green body at 1400 ℃ for 5 hours, roasting at 2400 ℃ and keeping the temperature for 10 hours, wherein the heating rate during heating is 10 ℃/min, and naturally cooling to room temperature after the heating is finished to obtain the refractory material.
Example 6:
a preparation process of a machined high-strength refractory material comprises the following steps:
step 1, weighing raw and auxiliary materials according to mass percentage, wherein 39% of aluminum oxide, 20% of chromium oxide, 15% of silicon oxide, 5% of calcium oxide, 3% of magnesium oxide, 1% of titanium oxide, 1% of yttrium oxide, 1% of niobium pentoxide and 15% of modified zirconia fiber, crushing the raw and auxiliary materials, carrying out magnetic separation treatment to remove ferromagnetic substances in the raw and auxiliary materials, then mixing the mixed raw materials with coal dust accounting for 8 wt% of the raw materials, uniformly mixing and grinding, spraying the mixed powder into a rotary kiln to sinter, heating to 230 ℃, keeping the temperature for 1.5 hours, heating to 600 ℃, keeping the temperature for 1 hour, heating to 1000 ℃, sintering for 3 hours, continuously rotating the rotary kiln in the sintering process, and obtaining material powder when the heating rate in the rotary kiln is 5 ℃/min;
wherein the particle size of the silicon oxide is 500nm, the purity is 95 wt%, the particle size of the aluminum oxide is 500nm, the purity is 98 wt%, and the modified zirconia fiber is prepared by the following steps: 50 parts of zirconia, 3 parts of calcium oxide and 1 part of sodium oxide are added, and the molar ratio of 400 parts of calcium oxide to 400 parts of sodium oxide is 1: 1, grinding for 15 hours by using absolute ethyl alcohol as grinding medium, calcining for 8 hours at the temperature of 1000 ℃, grinding, cleaning and drying after calcining and cooling
Step 2, ball-milling and mixing the material powder treated in the step 1 in absolute ethyl alcohol of which the weight is 3 times that of the material powder for 5 hours, wherein the ball-milling rotating speed during ball-milling is 2300rpm, and drying the material powder after ball-milling and mixing;
step 3, dry-pressing and molding the material powder treated in the step 2 under the pressure of 150MPa, and uniformly spraying 0.1mol/L sodium carbonate aqueous solution with the mass of 10% of the raw materials in the molding process to finally prepare a refractory material green body;
and 4, sintering the molded refractory material green body at 1400 ℃ for 5 hours, roasting at 2400 ℃ and keeping the temperature for 10 hours, wherein the heating rate during heating is 10 ℃/min, and naturally cooling to room temperature after the heating is finished to obtain the refractory material.
Example 7:
a preparation process of a machined high-strength refractory material comprises the following steps:
step 1, weighing raw and auxiliary materials according to mass percentage, wherein 30% of aluminum oxide, 20% of chromium oxide, 15% of silicon oxide, 10% of calcium oxide, 5% of magnesium oxide, 2% of titanium oxide, 2% of yttrium oxide, 1% of niobium pentoxide and 15% of modified zirconia fiber, crushing the raw and auxiliary materials, carrying out magnetic separation treatment to remove ferromagnetic substances in the raw and auxiliary materials, then mixing the mixed raw materials with coal dust accounting for 8 wt% of the raw materials, uniformly mixing and grinding, spraying the mixed powder into a rotary kiln to sinter, heating to 230 ℃, keeping the temperature for 1.5 hours, heating to 600 ℃, keeping the temperature for 1 hour, heating to 1000 ℃, sintering for 3 hours, continuously rotating the rotary kiln in the sintering process, and obtaining material powder when the heating rate in the rotary kiln is 5 ℃/min;
wherein the particle size of the silicon oxide is 500nm, the purity is 95 wt%, the particle size of the aluminum oxide is 500nm, the purity is 98 wt%, and the modified zirconia fiber is prepared by the following steps: 50 parts of zirconia, 3 parts of calcium oxide and 1 part of sodium oxide are added, and the molar ratio of 400 parts of calcium oxide to 400 parts of sodium oxide is 1: 1, grinding for 15 hours by using absolute ethyl alcohol as grinding medium, calcining for 8 hours at the temperature of 1000 ℃, grinding, cleaning and drying after calcining and cooling
Step 2, ball-milling and mixing the material powder treated in the step 1 in absolute ethyl alcohol of which the weight is 3 times that of the material powder for 5 hours, wherein the ball-milling rotating speed during ball-milling is 2300rpm, and drying the material powder after ball-milling and mixing;
step 3, dry-pressing and molding the material powder treated in the step 2 under the pressure of 150MPa, and uniformly spraying 0.1mol/L sodium carbonate aqueous solution with the mass of 10% of the raw materials in the molding process to finally prepare a refractory material green body;
and 4, sintering the molded refractory material green body at 1400 ℃ for 5 hours, roasting at 2400 ℃ and keeping the temperature for 10 hours, wherein the heating rate during heating is 10 ℃/min, and naturally cooling to room temperature after the heating is finished to obtain the refractory material.
Example 8:
a preparation process of a machined high-strength refractory material comprises the following steps:
step 1, weighing raw and auxiliary materials according to mass percentage, wherein 30% of aluminum oxide, 23% of chromium oxide, 22% of silicon oxide, 5% of calcium oxide, 5% of magnesium oxide, 2% of titanium oxide, 2% of yttrium oxide, 1% of niobium pentoxide and 15% of modified zirconia fiber, crushing the raw and auxiliary materials, carrying out magnetic separation treatment to remove ferromagnetic substances in the raw and auxiliary materials, then mixing the mixed raw materials with coal dust accounting for 8 wt% of the raw materials, uniformly mixing and grinding, spraying the mixed powder into a rotary kiln to sinter, heating to 230 ℃, keeping the temperature for 1.5 hours, heating to 600 ℃, keeping the temperature for 1 hour, heating to 1000 ℃, sintering for 3 hours, continuously rotating the rotary kiln in the sintering process, and obtaining material powder when the heating rate in the rotary kiln is 5 ℃/min;
wherein the particle size of the silicon oxide is 500nm, the purity is 95 wt%, the particle size of the aluminum oxide is 500nm, the purity is 98 wt%, and the modified zirconia fiber is prepared by the following steps: 50 parts of zirconia, 3 parts of calcium oxide and 1 part of sodium oxide are added, and the molar ratio of 400 parts of calcium oxide to 400 parts of sodium oxide is 1: 1, grinding for 15 hours by using absolute ethyl alcohol as grinding medium, calcining for 8 hours at the temperature of 1000 ℃, grinding, cleaning and drying after calcining and cooling
Step 2, ball-milling and mixing the material powder treated in the step 1 in absolute ethyl alcohol of which the weight is 3 times that of the material powder for 5 hours, wherein the ball-milling rotating speed during ball-milling is 2300rpm, and drying the material powder after ball-milling and mixing;
step 3, dry-pressing and molding the material powder treated in the step 2 under the pressure of 150MPa, and uniformly spraying 0.1mol/L sodium carbonate aqueous solution with the mass of 10% of the raw materials in the molding process to finally prepare a refractory material green body;
and 4, sintering the molded refractory material green body at 1400 ℃ for 5 hours, roasting at 2400 ℃ and keeping the temperature for 10 hours, wherein the heating rate during heating is 10 ℃/min, and naturally cooling to room temperature after the heating is finished to obtain the refractory material.
Example 9:
the machined high strength refractories made according to the manufacturing process described in examples 1-8 were tested several times for the properties of the materials made according to the manufacturing process described in examples 1-8, and the results were as follows:
the test result shows that the machined high-strength refractory material is more compact, has good heat resistance and toughness, does not generate a large amount of cracks in a use environment of rapid cooling and rapid heating, belongs to a qualified refractory material, and can meet the requirements of industrial production.
The invention is applied to the technical field of refractory materials, adjusts the formula of the refractory materials, adjusts the mass percent of each raw and auxiliary material in the formula, crushes the raw and auxiliary materials according to the adding sequence, grinds and stirs the raw and auxiliary materials, adds magnetic separation treatment, can remove ferromagnetic substances, improves the purity of the materials, finally uses a step-by-step heating mode to gradually heat in the heating process, improves the hardness of the refractory materials, does not generate a large amount of cracks under the use environment of rapid cooling and rapid heating, has long service life of products, and can better meet the requirements of industrial production.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (10)
1. A preparation process of a machined high-strength refractory material is characterized by comprising the following steps:
step 1, weighing raw and auxiliary materials according to mass percentage, wherein the raw and auxiliary materials comprise aluminum oxide, chromium oxide, silicon oxide, calcium oxide, magnesium oxide, titanium oxide, yttrium oxide, niobium pentoxide and modified zirconia fiber, and crushing, mixing, grinding and presintering the raw and auxiliary materials to obtain material powder;
step 2, ball-milling and mixing the material powder treated in the step 1 in absolute ethyl alcohol of which the weight is 2-3 times that of the material powder for 3-5 hours, and drying the material powder after ball-milling and mixing;
step 3, dry-pressing and molding the material powder treated in the step 2 under the pressure of 100-150 MPa, uniformly spraying a sodium carbonate aqueous solution in the molding process, wherein the concentration of the sodium carbonate aqueous solution is 0.05-0.1 mol/L, and the mass of the sodium carbonate aqueous solution is 6-10% of the mass of the material powder, and finally preparing a refractory material green body;
and 4, sintering the molded refractory material green body at 1200-1400 ℃ for 3-5 hours, roasting at 2200-2400 ℃ for 8-10 hours, and naturally cooling to room temperature after roasting is completed to obtain the refractory material.
2. The preparation process of the machined high-strength refractory material according to claim 1, wherein the raw materials and auxiliary materials in the step 1 comprise the following components in percentage by mass:
30-50% of aluminum oxide;
20-30% of chromium oxide;
15-40% of silicon oxide;
5-10% of calcium oxide;
3-5% of magnesium oxide;
1-2% of titanium oxide;
1-2% of yttrium oxide;
0.5-1% of niobium pentoxide;
10-15% of modified zirconia fiber.
3. The process of claim 2, wherein the modified zirconia fiber is prepared by the steps of: 50 parts of zirconia, 3 parts of calcium oxide and 1 part of sodium oxide are added, and the molar ratio of 400 parts of calcium oxide to 400 parts of sodium oxide is 1: 1, grinding for 10-15 hours by taking absolute ethyl alcohol as a grinding medium, calcining for 5-8 hours at 800-1000 ℃, grinding, cleaning and drying after calcining and cooling.
4. The process according to claim 2, wherein the silica has a particle size of 200 to 500nm and a purity of 95 wt%.
5. The process for preparing a machined high-strength refractory material according to claim 2, wherein the alumina has a particle size of 100 to 500nm and a purity of 98 wt%.
6. The process of claim 1, wherein in step 1, the raw and auxiliary materials are crushed and then subjected to magnetic separation to remove ferromagnetic substances.
7. The process for preparing a machined high-strength refractory material according to claim 1, wherein the specific steps of mixing, grinding and pre-sintering the raw materials in the step 1 are as follows: mixing and grinding the raw materials, mixing the raw materials with coal powder accounting for 6-8 wt% of the weight of the raw materials, uniformly mixing and grinding, spraying the mixed powder into a rotary kiln for sintering, heating to 180-230 ℃, preserving heat for 1-1.5 hours, heating to 550-600 ℃, preserving heat for 0.5-1 hour, heating to 900-1000 ℃, sintering for 2-3 hours, and continuously rotating the rotary kiln in the sintering process.
8. The process according to claim 7, wherein the temperature rise rate during the temperature rise in the rotary kiln is 3-5 ℃/min.
9. The process for preparing a machined high-strength refractory according to claim 1, wherein the ball milling rotation speed in the ball milling in the step 2 is 1800-2300 rpm.
10. The process for preparing a machined high-strength refractory according to claim 1, wherein in the step 4, the temperature rise rate during temperature rise is 5-10 ℃/min.
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Application publication date: 20220422 |