A refractory aluminum-magnesium spinel brick material and preparation method thereof

Abstract

The present invention relates to the technical field of spinel bricks, and in particular to a refractory aluminum-magnesium spinel brick material and a preparation method thereof, comprising the following raw materials in parts by weight: 35-40 parts of fused magnesia, 20-30 parts of aluminum-magnesium spinel, 10-15 parts of an external additive modified by mullite, 7-11 parts of a stabilizer, 6-10 parts of a high-aluminum micropowder, and 3-6 parts of an external binder. The aluminum-magnesium spinel brick material of the present invention adopts fused magnesia, aluminum-magnesium spinel with high-aluminum micropowder and an external binder, and the external additive modified by mullite and the stabilizer added at the same time are coordinated and synergistic with each other, so that the strength, wear resistance and thermal insulation of the obtained aluminum-magnesium spinel brick material are coordinated and improved, and the product has remarkable fire resistance and alkali corrosion resistance stability effects.

Description

Technical Field

[0001] The present invention relates to the technical field of spinel bricks, and in particular to a refractory alumina-magnesia spinel brick material and a preparation method thereof. Background Art

[0002] The cement rotary kiln is an important equipment in cement production. The lining material of the high-temperature zone of the cement rotary kiln is the key factor to ensure the stable operation of the kiln body in a high-temperature environment. Magnesium-iron-aluminum spinel material is currently considered to be the best material to replace magnesia-chrome bricks for the firing zone of the cement rotary kiln.

[0003] Existing spinel brick materials have poor compressive strength performance, and the products also have poor wear resistance and thermal insulation. It is difficult to achieve coordinated improvements in strength, wear resistance and thermal insulation. In addition, the products have poor fire resistance and alkali corrosion resistance, which limits the product's utilization efficiency. Based on this, the present invention further improves it. Summary of the Invention

[0004] In view of the defects of the prior art, the purpose of the present invention is to provide a refractory alumina-magnesia spinel brick material and a preparation method thereof to solve the problems raised in the above background technology.

[0005] The present invention solves the technical problem by adopting the following technical solutions:

[0006] The present invention provides a refractory alumina-magnesia spinel brick material, comprising the following raw materials in parts by weight:

[0007] 35-40 parts of fused magnesia, 20-30 parts of aluminum-magnesium spinel, 10-15 parts of an external additive modified by mullite, 7-11 parts of a stabilizing material, 6-10 parts of high-aluminum micropowder, and 3-6 parts of an external binder; the preparation method of the external additive modified by mullite is as follows: S01, preparation of a modifier modified by mullite;

[0008] S02, preparing a 5-8% by mass solution of sodium dodecylbenzenesulfonate and a 6-9% by mass solution of sodium silicate;

[0009] Add 3-5 parts by weight of barium zirconate and 2-3 parts by weight of strontium titanate to 5-8 parts by weight of sodium dodecylbenzenesulfonate solution and stir evenly to obtain a co-adjusting solution;

[0010] S03, adding 2-3 parts by weight of basalt fiber and 1-3 parts by weight of boron nitride to 4-7 parts by weight of sodium silicate solution and blending them evenly to obtain an admixture;

[0011] The admixture and the auxiliary liquid are mixed evenly in a weight ratio of 3:5 to obtain an external auxiliary functional liquid;

[0012] S04, the modifier and the external functional liquid mixed with mullite are mixed and ball-milled in a weight ratio of 5: (2-3), the ball milling speed is 1000-1500r / min, the ball milling is carried out for 1-2h, and after the ball milling is completed, the mixture is filtered and dried to obtain the external additive modified with mullite; the preparation method of the stabilized material is as follows:

[0013] S101: 2-4 parts by weight of titanium oxide, 3-5 parts by weight of wollastonite, and 2-3 parts by weight of volcanic ash are mixed and sintered for 1-2 hours at a sintering temperature of 300-350° C., to obtain a sintered body;

[0014] 5-8 parts by weight of dopamine hydrochloride solution and 4-7 parts by weight of the sintered body are uniformly blended to obtain a modified solution;

[0015] S102: preheating the expanded vermiculite at 60-65° C. for 1-2 hours, ultrasonically treating the preheated expanded vermiculite and the modified liquid in a weight ratio of 3:5. After the ultrasonic treatment is completed, washing, filtering, and drying are performed to obtain a stabilized material.

[0016] Preferably, the particle size of the fused magnesia is 0.2-0.5 mm;

[0017] The mass fraction of aluminum oxide in the aluminum-magnesium spinel is 75-80%, the total mass fraction of aluminum oxide and magnesium oxide is ≥98%, and the particle size of the aluminum-magnesium spinel is 0.05-0.07 mm;

[0018] The particle size of high-alumina micropowder is 0.4-0.6 μm; the added binder is paper pulp.

[0019] The mullite-modified external additive is prepared by mixing and ball-milling the mullite-modified modifier with an external functional liquid. The mullite-modified modifier is mixed and stirred with a mullite sintering agent and a doping liquid. The mullite in the mullite sintering agent is sintered and improved with boron oxide and lanthanum oxide. With mullite as the matrix, the high temperature resistance of the system is enhanced. The coordination of boron oxide and lanthanum oxide fills the system structure, further enhancing the performance coordination and performance stability of the system.

[0020] Preferably, the basalt fiber has a diameter of 10-15 μm and a length of 0.5-0.8 mm.

[0021] Preferably, the specific preparation method of the modifier mixed with mullite is:

[0022] S01a: adding 3-5 parts by weight of titanium carbide, 4-6 parts by weight of double-walled carbon nanotubes, and 1-2 parts by weight of silane coupling agent KH550 to 5-8 parts by weight of a 4-6% cerium nitrate solution and uniformly blending to obtain a doping solution;

[0023] S01b: Mullite, boron oxide and lanthanum oxide are uniformly mixed in a weight ratio of (5-8): (3-4): 2, and then sintered to obtain a mullite sintered preparation;

[0024] The mullite sintered preparation and the added liquid were mixed and stirred thoroughly in a weight ratio of 3:5, and then filtered and dried to obtain a modifier mixed with mullite.

[0025] Preferably, the double-walled carbon nanotubes have a diameter of 3-5 nm, a length of 1-2 μm, and a specific surface area of ​​380-400 μm. 2 / g; the sintering temperature of the sintering treatment is 750-800℃, and the sintering time is 1-2h.

[0026] The double-walled carbon nanotubes in the doping liquid are combined with cerium nitrate solution, titanium carbide and silane coupling agent KH550. Through the coordination and optimization of the raw materials, the carbon nanotubes are used as the matrix raw material to enhance the interfacial effect of the system. The coordination of cerium nitrate solution and titanium carbide can further enhance the coordination effect between the doping liquid and the mullite sintering agent. The resulting modifier doped with mullite not only enhances the interfacial properties of the system and improves the interfacial connectivity between the raw materials, but also optimizes the performance coordination and performance stability of the system.

[0027] The external auxiliary functional liquid is combined with the auxiliary liquid through an external additive. The external additive adopts sodium silicate solution combined with basalt fiber and boron nitride raw materials. At the same time, the barium zirconate, strontium titanate and sodium dodecylbenzene sulfonate solution in the auxiliary liquid are further blended and coordinated. The needle-like structure of the basalt fiber and the sheet-like structure of the boron nitride are further blended with barium zirconate and strontium titanate to further strengthen the system structure. At the same time, the external auxiliary functional liquid can better coordinate with the modifier mixed with mullite, and the external additive modified by mixing mullite in the system further optimizes the performance coordination and performance stability of the system.

[0028] Preferably, the mass fraction of the dopamine hydrochloride solution is 4-7%; the ultrasonic power of the ultrasonic treatment is 350-400W, and the ultrasonic treatment is performed for 1 hour.

[0029] The stabilizing material is made of expanded vermiculite after being preheated and then ultrasonically treated with a modifying liquid. The modifying liquid is made by uniformly blending a dopamine hydrochloride solution and a sintered body. The sintered body is further blended with titanium oxide, wollastonite and volcanic ash, and then treated with sintering improvement. Titanium oxide, wollastonite and volcanic ash are further supplemented into the system, so that the prepared stabilizing material is further coordinated with the external additive modified by mullite, thereby further coordinating and improving the performance of the product and further optimizing and improving the stability of the product.

[0030] The present invention also provides a method for preparing a refractory alumina-magnesia spinel brick material, comprising the following steps:

[0031] The raw materials are weighed according to parts by weight, and the raw materials are molded at a molding pressure of 100-150 MPa for 1-2 hours, and then sintered. After the sintering is completed, a refractory alumina-magnesia spinel brick material is obtained.

[0032] Preferably, the sintering temperature of the sintering treatment is 1500-1530° C., and the sintering time is 5-8 hours.

[0033] Compared with the prior art, the present invention has the following beneficial effects:

[0034] The aluminum-magnesium spinel brick material of the present invention adopts fused magnesia sand, aluminum-magnesium spinel combined with high-aluminum micropowder and external binder, and the added external additive modified by mullite and stabilizer are coordinated and synergistic with each other. The strength, wear resistance and thermal insulation of the obtained aluminum-magnesium spinel brick material are coordinated and improved, and the product has significant fire resistance and alkali corrosion resistance stability. DETAILED DESCRIPTION

[0035] The following is a clear and complete description of the technical solutions in the embodiments of the present invention in conjunction with specific embodiments. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative efforts are within the scope of protection of the present invention.

[0036] A refractory alumina-magnesia spinel brick material of this embodiment includes the following raw materials in parts by weight:

[0037] 35-40 parts of fused magnesia, 20-30 parts of aluminum-magnesium spinel, 10-15 parts of external additive modified by mullite, 7-11 parts of stabilizer, 6-10 parts of high-aluminum micropowder, and 3-6 parts of external binder.

[0038] The particle size of the fused magnesia in this embodiment is 0.2-0.5 mm;

[0039] The mass fraction of aluminum oxide in the aluminum-magnesium spinel is 75-80%, the total mass fraction of aluminum oxide and magnesium oxide is ≥98%, and the particle size of the aluminum-magnesium spinel is 0.05-0.07 mm;

[0040] The particle size of high-alumina micropowder is 0.4-0.6 μm; the added binder is paper pulp.

[0041] The preparation method of the mullite-modified external additive of this embodiment is as follows:

[0042] S01, preparation of a modifier mixed with mullite;

[0043] S02, preparing a 5-8% by mass solution of sodium dodecylbenzenesulfonate and a 6-9% by mass solution of sodium silicate;

[0044] Add 3-5 parts by weight of barium zirconate and 2-3 parts by weight of strontium titanate to 5-8 parts by weight of sodium dodecylbenzenesulfonate solution and stir evenly to obtain a co-adjusting solution;

[0045] S03, adding 2-3 parts by weight of basalt fiber and 1-3 parts by weight of boron nitride to 4-7 parts by weight of sodium silicate solution and blending them evenly to obtain an admixture;

[0046] The admixture and the auxiliary liquid are mixed evenly in a weight ratio of 3:5 to obtain an external auxiliary functional liquid;

[0047] S04, the modifier blended with mullite and the external functional liquid are mixed and ball-milled in a weight ratio of 5:(2-3), the ball milling speed is 1000-1500 r / min, the ball milling is carried out for 1-2 hours, and after the ball milling is completed, the mixture is filtered and dried to obtain the external additive modified with mullite.

[0048] The basalt fiber of this embodiment has a diameter of 10-15 μm and a length of 0.5-0.8 mm.

[0049] The specific preparation method of the modifier mixed with mullite in this embodiment is:

[0050] S01a: adding 3-5 parts by weight of titanium carbide, 4-6 parts by weight of double-walled carbon nanotubes, and 1-2 parts by weight of silane coupling agent KH550 to 5-8 parts by weight of a 4-6% cerium nitrate solution and uniformly blending to obtain a doping solution;

[0051] S01b: Mullite, boron oxide and lanthanum oxide are uniformly mixed in a weight ratio of (5-8): (3-4): 2, and then sintered to obtain a mullite sintered preparation;

[0052] The mullite sintered preparation and the added liquid were mixed and stirred thoroughly in a weight ratio of 3:5, and then filtered and dried to obtain a modifier mixed with mullite.

[0053] The double-walled carbon nanotubes of this embodiment have a diameter of 3-5 nm, a length of 1-2 μm, and a specific surface area of ​​380-400 m 2 / g; the sintering temperature of the sintering treatment is 750-800℃, and the sintering time is 1-2h.

[0054] The preparation method of the stabilizing material of this embodiment is:

[0055] S101: 2-4 parts by weight of titanium oxide, 3-5 parts by weight of wollastonite, and 2-3 parts by weight of volcanic ash are mixed and sintered for 1-2 hours at a sintering temperature of 300-350° C., to obtain a sintered body;

[0056] 5-8 parts by weight of dopamine hydrochloride solution and 4-7 parts by weight of the sintered body are uniformly blended to obtain a modified solution;

[0057] S102: preheating the expanded vermiculite at 60-65° C. for 1-2 hours, ultrasonically treating the preheated expanded vermiculite and the modified liquid in a weight ratio of 3:5. After the ultrasonic treatment is completed, washing, filtering, and drying are performed to obtain a stabilized material.

[0058] The mass fraction of the dopamine hydrochloride solution in this embodiment is 4-7%; the ultrasonic power of the ultrasonic treatment is 350-400W, and the ultrasonic treatment is performed for 1 hour.

[0059] A method for preparing a refractory alumina-magnesia spinel brick material according to this embodiment includes the following steps:

[0060] The raw materials are weighed according to parts by weight, and the raw materials are molded at a molding pressure of 100-150 MPa for 1-2 hours, and then sintered. After the sintering is completed, a refractory alumina-magnesia spinel brick material is obtained.

[0061] The sintering temperature of the sintering process in this embodiment is 1500-1530° C., and the sintering time is 5-8 hours.

[0062] Example 1.

[0063] A refractory alumina-magnesia spinel brick material of this embodiment includes the following raw materials in parts by weight:

[0064] 35 parts of fused magnesia, 20 parts of aluminum-magnesium spinel, 10 parts of external additive modified by mullite, 7 parts of stabilizer, 6 parts of high-aluminum micropowder, and 3 parts of external binder.

[0065] The particle size of the fused magnesia in this embodiment is 0.2 mm;

[0066] The mass fraction of aluminum oxide in the aluminum-magnesium spinel is 75%, the total mass fraction of aluminum oxide and magnesium oxide is ≥98%, and the particle size of the aluminum-magnesium spinel is 0.05 mm;

[0067] The particle size of high-alumina micropowder is 0.4 μm; the added binder is paper pulp.

[0068] The preparation method of the mullite-modified external additive of this embodiment is as follows:

[0069] S01, preparation of a modifier mixed with mullite;

[0070] S02, preparing a 5% by mass solution of sodium dodecylbenzenesulfonate and a 6% by mass solution of sodium silicate;

[0071] 3 parts by weight of barium zirconate and 2 parts by weight of strontium titanate were added to 5 parts by weight of sodium dodecylbenzenesulfonate solution and stirred to obtain a co-adjusting solution;

[0072] S03, adding 2 parts by weight of basalt fiber and 1 part by weight of boron nitride to 4 parts by weight of sodium silicate solution and blending them evenly to obtain an admixture;

[0073] The admixture and the auxiliary liquid are mixed evenly in a weight ratio of 3:5 to obtain an external auxiliary functional liquid;

[0074] S04, the modifier mixed with mullite and the external functional liquid are mixed and ball-milled in a weight ratio of 5:2, the ball milling speed is 1000 r / min, the ball milling is carried out for 1 hour, and after the ball milling is completed, the mixture is filtered and dried to obtain the external additive modified with mullite.

[0075] The basalt fiber of this embodiment has a diameter of 10 μm and a length of 0.5 mm.

[0076] The specific preparation method of the modifier mixed with mullite in this embodiment is:

[0077] S01a: adding 3 parts by weight of titanium carbide, 4 parts of double-walled carbon nanotubes and 1 part by weight of silane coupling agent KH550 to 5 parts by weight of a 4% cerium nitrate solution and blending them evenly to obtain a doping solution;

[0078] S01b: Mullite, boron oxide and lanthanum oxide are uniformly mixed in a weight ratio of 5:3:2, and then sintered to obtain a mullite sintered mixture.

[0079] The mullite sintered preparation and the added liquid were mixed and stirred thoroughly in a weight ratio of 3:5, and then filtered and dried to obtain a modifier mixed with mullite.

[0080] The double-walled carbon nanotubes in this embodiment have a diameter of 3 nm, a length of 1 μm, and a specific surface area of ​​380 m 2 / g; the sintering temperature of the sintering treatment is 750℃ and the sintering time is 1h.

[0081] The preparation method of the stabilizing material of this embodiment is:

[0082] S101: 2 parts by weight of titanium oxide, 3 parts by weight of wollastonite, and 2 parts by weight of volcanic ash are mixed and sintered for 1 hour at a sintering temperature of 300° C., to obtain a sintered body;

[0083] 5 parts by weight of dopamine hydrochloride solution and 4 parts by weight of the sintered body are uniformly mixed to obtain a modified solution;

[0084] S102: preheating the expanded vermiculite at 60° C. for 1 hour, ultrasonically treating the preheated expanded vermiculite and the modified liquid in a weight ratio of 3:5. After the ultrasonic treatment is completed, washing, filtering, and drying are performed to obtain a stabilized material.

[0085] The mass fraction of the dopamine hydrochloride solution in this embodiment is 4%; the ultrasonic power of the ultrasonic treatment is 350 W, and the ultrasonic treatment is performed for 1 hour.

[0086] A method for preparing a refractory alumina-magnesia spinel brick material according to this embodiment includes the following steps:

[0087] The raw materials are weighed according to parts by weight, and the raw materials are molded at a molding pressure of 100 MPa for 1 hour, and then sintered. After the sintering is completed, a refractory aluminum-magnesium spinel brick material is obtained.

[0088] The sintering temperature of the sintering process in this embodiment is 1500° C., and the sintering time is 5 hours.

[0089] Example 2.

[0090] A refractory alumina-magnesia spinel brick material of this embodiment includes the following raw materials in parts by weight:

[0091] 40 parts of fused magnesia, 30 parts of aluminum-magnesium spinel, 15 parts of external additive modified by mullite, 11 parts of stabilizer, 10 parts of high-aluminum micropowder, and 6 parts of external binder.

[0092] The particle size of the fused magnesia in this embodiment is 0.5 mm;

[0093] The mass fraction of aluminum oxide in the aluminum-magnesium spinel is 80%, the total mass fraction of aluminum oxide and magnesium oxide is ≥98%, and the particle size of the aluminum-magnesium spinel is 0.07 mm;

[0094] The particle size of high-alumina micropowder is 0.6 μm; the added binder is paper pulp.

[0095] The preparation method of the mullite-modified external additive of this embodiment is as follows:

[0096] S01, preparation of a modifier mixed with mullite;

[0097] S02, preparing 8% by mass of sodium dodecylbenzenesulfonate solution and 9% by mass of sodium silicate solution;

[0098] 5 parts by weight of barium zirconate and 3 parts by weight of strontium titanate were added to 8 parts by weight of sodium dodecylbenzenesulfonate solution and stirred to obtain a co-adjusting solution;

[0099] S03, adding 3 parts by weight of basalt fiber and 3 parts by weight of boron nitride to 7 parts by weight of sodium silicate solution and blending them evenly to obtain an admixture;

[0100] The admixture and the auxiliary liquid are mixed evenly in a weight ratio of 3:5 to obtain an external auxiliary functional liquid;

[0101] S04, the modifier mixed with mullite and the external functional liquid are mixed in a weight ratio of 5:3 and ball-milled at a ball milling speed of 1500 r / min for 2 h. After the ball milling is completed, the mixture is filtered and dried to obtain the external additive modified with mullite.

[0102] The basalt fiber of this embodiment has a diameter of 15 μm and a length of 0.8 mm.

[0103] The specific preparation method of the modifier mixed with mullite in this embodiment is:

[0104] S01a: adding 5 parts by weight of titanium carbide, 6 parts of double-walled carbon nanotubes and 2 parts by weight of silane coupling agent KH550 to 8 parts by weight of 6% cerium nitrate solution and blending them evenly to obtain a doping solution;

[0105] S01b: Mullite, boron oxide and lanthanum oxide are uniformly mixed in a weight ratio of 8:4:2, and then sintered to obtain a mullite sintered mixture.

[0106] The mullite sintered preparation and the added liquid were mixed and stirred thoroughly in a weight ratio of 3:5, and then filtered and dried to obtain a modifier mixed with mullite.

[0107] The double-walled carbon nanotubes in this embodiment have a diameter of 5 nm, a length of 2 μm, and a specific surface area of ​​400 m 2 / g; the sintering temperature of the sintering treatment is 800℃ and the sintering time is 2h.

[0108] The preparation method of the stabilizing material of this embodiment is:

[0109] S101: 4 parts by weight of titanium oxide, 5 parts by weight of wollastonite, and 3 parts by weight of volcanic ash are mixed and sintered for 2 hours at a sintering temperature of 350° C., to obtain a sintered body;

[0110] 8 parts by weight of dopamine hydrochloride solution and 7 parts by weight of the sintered body are uniformly blended to obtain a modified solution;

[0111] S102: preheating the expanded vermiculite at 65° C. for 2 h, ultrasonically treating the preheated expanded vermiculite and the modified liquid in a weight ratio of 3:5. After the ultrasonic treatment is completed, washing, filtering, and drying are performed to obtain a stabilized material.

[0112] The mass fraction of the dopamine hydrochloride solution in this embodiment is 7%; the ultrasonic treatment power is 400 W, and the ultrasonic treatment is performed for 1 hour.

[0113] A method for preparing a refractory alumina-magnesia spinel brick material according to this embodiment includes the following steps:

[0114] The raw materials are weighed according to parts by weight, and the raw materials are molded at a molding pressure of 150 MPa for 2 hours, and then sintered. After the sintering is completed, a refractory aluminum-magnesium spinel brick material is obtained.

[0115] The sintering temperature of the sintering process in this embodiment is 1530° C., and the sintering time is 8 hours.

[0116] Example 3.

[0117] A refractory alumina-magnesia spinel brick material of this embodiment includes the following raw materials in parts by weight:

[0118] 37.5 parts of fused magnesia, 25 parts of aluminum-magnesium spinel, 12.5 parts of external additive modified by mullite, 9 parts of stabilizer, 8 parts of high-aluminum micropowder, and 4.5 parts of external binder.

[0119] The particle size of the fused magnesia in this embodiment is 0.35 mm;

[0120] The mass fraction of aluminum oxide in the aluminum-magnesium spinel is 78.5%, the total mass fraction of aluminum oxide and magnesium oxide is ≥98%, and the particle size of the aluminum-magnesium spinel is 0.06 mm;

[0121] The particle size of high-alumina micropowder is 0.5 μm; the added binder is paper pulp.

[0122] The preparation method of the mullite-modified external additive of this embodiment is as follows:

[0123] S01, preparation of a modifier mixed with mullite;

[0124] S02, preparing a 6.5% by mass solution of sodium dodecylbenzenesulfonate and a 7.5% by mass solution of sodium silicate;

[0125] 4 parts by weight of barium zirconate and 2.5 parts by weight of strontium titanate were added to 6.5 parts by weight of sodium dodecylbenzenesulfonate solution and stirred to obtain a co-adjusting solution;

[0126] S03, adding 2.5 parts by weight of basalt fiber and 2 parts by weight of boron nitride to 5.5 parts by weight of sodium silicate solution and blending them evenly to obtain an admixture;

[0127] The admixture and the auxiliary liquid are mixed evenly in a weight ratio of 3:5 to obtain an external auxiliary functional liquid;

[0128] S04, the modifier mixed with mullite and the external functional liquid are mixed and ball-milled in a weight ratio of 5:2.5, the ball milling speed is 1250 r / min, the ball milling is carried out for 1.5 hours, and after the ball milling is completed, the mixture is filtered and dried to obtain the external additive modified with mullite.

[0129] The basalt fiber of this embodiment has a diameter of 12.5 μm and a length of 0.65 mm.

[0130] The specific preparation method of the modifier mixed with mullite in this embodiment is:

[0131] S01a: 4 parts by weight of titanium carbide, 5 parts by weight of double-walled carbon nanotubes, and 1.5 parts by weight of silane coupling agent KH550 are added to 6.5 parts by weight of a 5% by mass cerium nitrate solution and mixed uniformly to obtain a doping solution;

[0132] S01b: Mullite, boron oxide and lanthanum oxide are uniformly mixed in a weight ratio of 6.5:3.5:2, and then sintered to obtain a mullite sintered mixture.

[0133] The mullite sintered preparation and the added liquid were mixed and stirred thoroughly in a weight ratio of 3:5, and then filtered and dried to obtain a modifier mixed with mullite.

[0134] The double-walled carbon nanotubes in this embodiment have a diameter of 4 nm, a length of 1.5 μm, and a specific surface area of ​​390 m 2 / g; the sintering temperature of the sintering treatment is 775℃, and the sintering time is 1.5h.

[0135] The preparation method of the stabilizing material of this embodiment is:

[0136] S101: 3 parts by weight of titanium oxide, 4 parts by weight of wollastonite, and 2.5 parts by weight of volcanic ash are mixed and sintered for 2 hours at a sintering temperature of 325° C., to obtain a sintered body;

[0137] 6.5 parts by weight of dopamine hydrochloride solution and 5.5 parts by weight of the sintered body are uniformly blended to obtain a modified solution;

[0138] S102: preheating the expanded vermiculite at 62.5° C. for 2 h, ultrasonically treating the preheated expanded vermiculite and the modified liquid in a weight ratio of 3:5. After the ultrasonic treatment is completed, washing, filtering, and drying are performed to obtain a stabilized material.

[0139] The mass fraction of the dopamine hydrochloride solution in this embodiment is 5.5%; the ultrasonic power of the ultrasonic treatment is 375W, and the ultrasonic treatment is performed for 1 hour.

[0140] A method for preparing a refractory alumina-magnesia spinel brick material according to this embodiment includes the following steps:

[0141] The raw materials are weighed according to parts by weight, and the raw materials are molded at a molding pressure of 125 MPa for 1.25 hours, and then sintered. After the sintering is completed, a refractory aluminum-magnesium spinel brick material is obtained.

[0142] The sintering temperature of the sintering process in this embodiment is 1515° C., and the sintering time is 6.5 hours.

[0143] Comparative Example 1.

[0144] The difference from Example 3 is that no mullite-modified external additive is added.

[0145] Comparative Example 2.

[0146] The difference from Example 3 is that no mullite-modified modifier is added in the preparation of the mullite-modified external additive.

[0147] Comparative Example 3.

[0148] The difference from Example 3 is that no external auxiliary functional liquid is added in the preparation of the mullite-modified external auxiliary agent.

[0149] Comparative Example 4.

[0150] The difference from Example 3 is that no admixture is added in the preparation of the external auxiliary functional liquid.

[0151] Comparative Example 5.

[0152] The difference from Example 3 is that basalt fiber and boron nitride are not added to the admixture.

[0153] Comparative Example 6.

[0154] The difference from Example 3 is that no auxiliary adjustment liquid is added in the preparation of the external auxiliary functional liquid.

[0155] Comparative Example 7.

[0156] The difference from Example 3 is that barium zirconate and strontium titanate are not added to the auxiliary adjustment liquid.

[0157] Comparative Example 8.

[0158] The difference from Example 3 is that no stabilizer is added.

[0159] Comparative Example 9.

[0160] The difference from Example 3 is that no preheated expanded vermiculite is added to the stabilizing material.

[0161] Comparative Example 10.

[0162] The difference from Example 3 is that no modifying liquid is added to the stabilizing material.

[0163] Comparative Example 11.

[0164] The difference from Example 3 is that no sintered body is added to the modifying liquid.

[0165] Comparative Example 12.

[0166] The difference from Example 3 is that no titanium oxide or wollastonite is added to the sintered body.

[0167] The products of Examples 1-3 and Comparative Examples 1-12 were subjected to conventional performance tests, and fire resistance and alkali corrosion resistance stability were tested (the products were placed under 5% sodium chloride salt spray conditions for 24 hours, and then treated under 120°C fire conditions for 12 hours, the above being one cycle, and the cycle was repeated 10 times);

[0168]

[0169] From comparative examples 1-12 and example 3, it can be seen that under normal conditions, the compressive strength, thermal insulation and wear resistance of the product of example 3 can be improved in a coordinated manner, with a compressive strength as high as 112 MPa, a thermal conductivity as low as 0.02 W / mk, and a wear resistance as low as 1.8 g / cm 3 , and the product has excellent performance stability under fire resistance and alkali corrosion resistance conditions;

[0170] The performance of the product showed a significant deterioration trend when no mullite-modified external additives or any of the stabilizers were added to the product. The performance of the product was most significant when the synergistic effect of the two was achieved.

[0171] The performance of the products tended to deteriorate when no modifier for mullite was added to the preparation of the mullite-modified external additive, no external functional liquid was added to the preparation of the mullite-modified external additive, and no admixture was added to the preparation of the external functional liquid.

[0172] In addition, when basalt fiber and boron nitride are not added to the admixture, no auxiliary adjustment liquid is added in the preparation of the external auxiliary functional liquid, and barium zirconate and strontium titanate are not added to the auxiliary adjustment liquid, the performance of the product also shows a trend of deterioration to varying degrees. The external auxiliary functional liquid prepared by combining the auxiliary adjustment liquid obtained by the specific process of the present invention and the external auxiliary functional liquid with the admixture, and the mullite-modified external auxiliary prepared by combining the mullite-adjusted modifier, have the most significant performance effects. The effects of other methods are not as obvious as those of the present invention.

[0173] No preheated expanded vermiculite was added to the stabilizing material, no modifying liquid was added to the stabilizing material, no sintered body was added to the modifying liquid, and no titanium oxide and wollastonite were added to the sintered body. The performance of the product also showed a trend of deterioration. The performance effect of the product was most significant when the modifying liquid obtained by combining the specific sintered body of the present invention and the stabilizing material made by combining the modifying liquid with preheated expanded vermiculite were used.

[0174] In addition, the product of the present invention is not treated with a modifier containing mullite, and the performance of the product has an obvious trend of deterioration. In this regard, the present invention further explores and processes it.

[0175] The specific preparation method of the modifier mixed with mullite is as follows:

[0176] S01a: 4 parts by weight of titanium carbide, 5 parts by weight of double-walled carbon nanotubes, and 1.5 parts by weight of silane coupling agent KH550 are added to 6.5 parts by weight of a 6% cerium nitrate solution and mixed uniformly to obtain a doping solution;

[0177] S01b: Mullite, boron oxide and lanthanum oxide are uniformly mixed in a weight ratio of 6.5:3.5:2, and then sintered to obtain a mullite sintered mixture.

[0178] The mullite sintered preparation and the added liquid were mixed and stirred thoroughly in a weight ratio of 3:5, and then filtered and dried to obtain a modifier mixed with mullite.

[0179] Experimental Example 1.

[0180] The same as Example 3, except that no doping liquid is added in the preparation of the modifier doped with mullite.

[0181] Experimental Example 2.

[0182] The same as Example 3, except that titanium carbide and double-walled carbon nanotubes are not added to the doping liquid.

[0183] Experimental Example 3.

[0184] The same as Example 3, except that the cerium nitrate solution and the silane coupling agent KH550 were not added to the doping solution.

[0185] Experimental Example 4.

[0186] The same as Example 3, the only difference is that the mullite sintering agent is not added.

[0187] Experimental Example 5.

[0188] The same as Example 3, the only difference is that boron oxide and lanthanum oxide are not added to the mullite sintering agent.

[0189] The product performance tests of Experimental Examples 1-5 are as follows:

[0190] It can be seen from Experimental Examples 1-5 that no mullite sintering agent is added in the preparation of the mullite-doped modifier. Among the preparation factors of the mullite-doped modifier, the performance of the product deteriorates most significantly. At the same time, no doping liquid is added in the preparation of the mullite-doped modifier, and the performance of the product also shows a relatively obvious deterioration trend. In addition, titanium carbide and double-walled carbon nanotubes are not added to the doping liquid, cerium nitrate solution and silane coupling agent KH550 are not added to the doping liquid, and boron oxide and lanthanum oxide are not added to the mullite sintering agent. The performance of the product shows a trend of deterioration to varying degrees. The mullite-doped modifier prepared by the doping liquid obtained by the specific method of the present invention and the mullite sintering agent has the most significant performance effect, and the use of other methods instead is not as obvious as the effect of the present invention.

[0191] It will be apparent to those skilled in the art that the present invention is not limited to the details of the exemplary embodiments described above and that the invention can be embodied in other specific forms without departing from the spirit or essential characteristics of the invention. Therefore, the embodiments should be considered in all respects as illustrative and non-restrictive, and the scope of the invention is defined by the appended claims rather than the foregoing description, and it is intended that all variations that come within the meaning and range of equivalents of the claims be embraced therein.

[0192] In addition, it should be understood that although this specification is described in terms of implementation methods, not every implementation method contains only one independent technical solution. This narrative method of the specification is only for the sake of clarity. Those skilled in the art should regard the specification as a whole. The technical solutions in each embodiment can also be appropriately combined to form other implementation methods that can be understood by those skilled in the art.

Claims

1. A refractory aluminum-magnesium spinel brick material, characterized in that: It includes the following raw materials in parts by weight: 35-40 parts of fused magnesia, 20-30 parts of aluminum-magnesium spinel, 10-15 parts of external additive modified by mullite, 7-11 parts of stabilizer, 6-10 parts of high-aluminum micropowder, and 3-6 parts of external binder; The preparation method of the mullite-modified external additive is as follows: S01, preparation of a modifier mixed with mullite; S02, preparing a 5-8% by mass solution of sodium dodecylbenzenesulfonate and a 6-9% by mass solution of sodium silicate; Add 3-5 parts by weight of barium zirconate and 2-3 parts by weight of strontium titanate to 5-8 parts by weight of sodium dodecylbenzenesulfonate solution and stir evenly to obtain a co-adjusting solution; S03, adding 2-3 parts by weight of basalt fiber and 1-3 parts by weight of boron nitride to 4-7 parts by weight of sodium silicate solution and blending them evenly to obtain an admixture; The admixture and the auxiliary liquid are mixed evenly in a weight ratio of 3:5 to obtain an external auxiliary functional liquid; S04, the modifier and the external functional liquid mixed with mullite are mixed and ball-milled in a weight ratio of 5: (2-3), the ball milling speed is 1000-1500 r / min, the ball milling is carried out for 1-2 hours, and after the ball milling is completed, the mixture is filtered and dried to obtain the external additive modified with mullite; The preparation method of the stabilized material is as follows: S101: 2-4 parts by weight of titanium oxide, 3-5 parts by weight of wollastonite, and 2-3 parts by weight of volcanic ash are mixed and sintered for 1-2 hours at a sintering temperature of 300-350° C., to obtain a sintered body; 5-8 parts by weight of dopamine hydrochloride solution and 4-7 parts by weight of the sintered body are uniformly blended to obtain a modified solution; S102: preheating the expanded vermiculite at 60-65° C. for 1-2 hours, ultrasonically treating the preheated expanded vermiculite and the modified liquid in a weight ratio of 3:

5. After the ultrasonic treatment is completed, washing, filtering, and drying are performed to obtain a stabilized material; The specific preparation method of the modifier mixed with mullite is as follows: S01a: adding 3-5 parts by weight of titanium carbide, 4-6 parts by weight of double-walled carbon nanotubes, and 1-2 parts by weight of silane coupling agent KH550 to 5-8 parts by weight of a 4-6% cerium nitrate solution and uniformly blending to obtain a doping solution; S01b: Mullite, boron oxide and lanthanum oxide are uniformly mixed in a weight ratio of (5-8): (3-4): 2, and then sintered to obtain a mullite sintered preparation; The mullite sintered preparation and the added liquid were mixed and stirred thoroughly in a weight ratio of 3:5, and then filtered and dried to obtain a modifier mixed with mullite.

2. A refractory alumina-magnesia spinel brick material according to claim 1, characterized in that: The particle size of the fused magnesia is 0.2-0.5 mm; The mass fraction of aluminum oxide in the aluminum-magnesium spinel is 75-80%, the total mass fraction of aluminum oxide and magnesium oxide is ≥98%, and the particle size of the aluminum-magnesium spinel is 0.05-0.07 mm; The particle size of high-alumina micropowder is 0.4-0.6 μm; the added binder is paper pulp.

3. The refractory alumina-magnesia spinel brick material according to claim 1, characterized in that: The basalt fiber has a diameter of 10-15 μm and a length of 0.5-0.8 mm.

4. The refractory alumina-magnesia spinel brick material according to claim 1, characterized in that: The diameter of double-walled carbon nanotubes is 3-5nm, the length is 1-2μm, and the specific surface area is 380-400m 2 / g; the sintering temperature of the sintering treatment is 750-800℃, and the sintering time is 1-2h.

5. The refractory alumina-magnesia spinel brick material according to claim 1, characterized in that: The mass fraction of the dopamine hydrochloride solution is 4-7%; the ultrasonic power of the ultrasonic treatment is 350-400W, and the ultrasonic treatment is performed for 1 hour.

6. The method for preparing a refractory alumina-magnesia spinel brick material according to any one of claims 1 to 5, characterized in that: The following steps are involved: The raw materials are weighed according to parts by weight, and the raw materials are molded at a molding pressure of 100-150 MPa for 1-2 hours, and then sintered. After the sintering is completed, a refractory alumina-magnesia spinel brick material is obtained.

7. The method for preparing a refractory alumina-magnesia spinel brick material according to claim 6, characterized in that: The sintering temperature of the sintering treatment is 1500-1530°C, and the sintering time is 5-8 hours.

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