Iron-containing corundum-high-iron mullite solid solution raw material and preparation method thereof

Through flotation technology and low-temperature liquid phase sintering method, the aluminum-silicon ratio is adjusted by sulfonic acid-phosphate bimodified cellulose, and a solid solution of iron-containing corundum-high-iron mullite was prepared, which solved the problem of low-grade bauxite resource utilization and improved the performance and resource utilization of refractory materials.

CN120483690AActive Publication Date: 2025-08-15SHANXI DAOER ALUMINUM CO LTD +2
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Patent Information

Application Number
CN202510774701.9
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-06-11
Publication Date
2025-08-15
Estimated Expiration
2045-06-11

AI Technical Summary

Technical Problem

The Al2O3 content in low grade bauxite is low, the SiO2 content is high, and Fe2O3 cannot be effectively removed, resulting in unstable quality of bauxite clinker, unable to meet the needs of high-efficiency refractory materials, and the medium and low grade ore resources are wasted and the environment is polluted.

Method used

The aluminum-silicon ratio is adjusted by flotation process, and sulfonic acid-phosphate bimodified cellulose as an inhibitor, combined with low-temperature liquid phase sintering method, iron-containing corundum-high-iron mullite solid solution raw materials are prepared. Through the combination of adjusters, inhibitors and collectors, uniform distribution and composition optimization of Fe2O3 and Al2O3 are achieved.

Benefits of technology

It improves the refractory resistance of the material, achieves efficient conversion of low-grade bauxite, reduces the generation of low melting point phase, and improves resource utilization and product added value.

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Abstract

The invention discloses an iron-containing corundum-high-iron mullite solid solution raw material and a preparation method thereof, and relates to the field of refractory materials, the iron-containing corundum-high-iron mullite solid solution raw material is obtained by selecting low-grade bauxite and carrying out crushing-flotation-sintering processes; comprising the following components: aluminum oxide, silicon dioxide, ferric oxide, titanium dioxide, calcium oxide and other impurities. Sulfonic acid-phosphoric acid double modified cellulose is used as an inhibitor in the flotation process to precisely regulate and control the Al / Si / Fe ratio, raw material homogenization and component optimization are achieved, microcosmic distribution of Fe2O3 and Al2O3 in flotation concentrate is more uniform, a homogeneous solid solution is formed during sintering, generation of a low-melting-point phase is avoided, and the refractoriness of the material is improved.
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Description

Technical Field

[0001] The invention relates to the field of refractory materials, and in particular to an iron-containing corundum-high-iron mullite solid solution raw material and a preparation method thereof. Background Art

[0002] Bauxite is a very important strategic resource. In recent years, with the rapid development of high-alumina bauxite clinker, existing problems have become increasingly exposed: (1) Excessive mining and consumption have led to the depletion of high-quality bauxite resources, while a large number of medium- and low-grade ores and crushed ores have been piled up and abandoned due to high processing costs and difficulties in development and utilization, resulting in huge waste of resources and environmental pollution; (2) The quality stability of calcined high-alumina bauxite clinker is poor, and it is unable to win the market with its quality. Looking at the development trend of refractory raw materials, many high-efficiency products with important uses are increasingly using high-quality synthetic raw materials.

[0003] Low-grade bauxite has a low Al2O3 content and a high SiO2 content. To economically and rationally utilize bauxite resources with a low to medium Al2O3 ratio, my country has conducted many small-scale flotation desiliconization experiments on diaspore since the 1970s. Finally, a variety of beneficiation process flows were identified, including stage grinding flotation desiliconization, stage grinding and stage beneficiation, selective agglomeration flotation, and selective grinding-selective agglomeration flotation. While the SiO2 content of the raw material after beneficiation can be effectively reduced, the Fe2O3 in the original ore cannot be effectively removed.

[0004] Therefore, this invention introduces flotation technology into the production of refractory raw materials. This process regulates the aluminum-silicon ratio in the material and homogenizes the material's composition. To address the issue of high Fe content in the raw materials, a low-temperature liquid-phase sintering method for preparing iron-rich mullite, based on the Fe2O3-Al2O3-SiO2 ternary system, was developed to overcome the low mullite conversion rate encountered in traditional solid-phase sintering processes. Summary of the Invention

[0005] In order to solve the above technical problems, the present invention provides an iron-containing corundum-high iron mullite solid solution raw material and a preparation method thereof.

[0006] The purpose of the present invention can be achieved through the following technical solutions:

[0007] A method for preparing an iron-containing corundum-high-iron mullite solid solution raw material comprises the following steps:

[0008] S1. Select low-grade bauxite as raw material and crush the raw material to obtain pre-treated particles;

[0009] S2. The pretreated particles are mixed and piled, and homogenized for 2-3 days using a flat-laying and straight-taking method to obtain homogenized ore particles;

[0010] S3, performing a flotation process on the homogenized ore particles, and filtering and drying the concentrate obtained by flotation to obtain concentrate particles;

[0011] S4. Add 3-5% by mass of lignin sulfonate to the concentrate particles, press them into a cylindrical body with a hydraulic press, perform gradient sintering on the cylindrical body, keep it warm for 4-6 hours, cool it to 200-400°C with the furnace, and then take it out of the furnace to obtain an iron-containing corundum-high iron mullite solid solution raw material.

[0012] Furthermore, the aluminum-silicon ratio of the low-grade bauxite in step S1 is 1.5-2.6:1, the aluminum oxide content is 40-60%, and the main mineral phase is diaspore.

[0013] Furthermore, the flotation process in step S3 includes: roughing 1-2 times, cleaning 1-2 times, and scavenging 1-2 times.

[0014] Furthermore, the flotation process in step S3 is:

[0015] (1) Grinding the homogenized ore particles to obtain a mineral powder material with a particle size of ≤0.075 mm, concentrating the mineral powder material to obtain a concentrated ore pulp with a mass concentration of 30-50%, sequentially adding 2-3 kg / t of a regulator, 0.5-1.2 kg / t of a depressant, and 0.8-1.5 kg / t of a collector, and performing a roughing operation to obtain a roughing concentrate and a roughing tailing;

[0016] (2) adding 0.1-0.3 kg / t of inhibitor and 0.05-0.1 kg / t of collector to the rougher concentrate, maintaining the pH at 9.0-9.5, and performing a primary concentration to obtain a concentrated concentrate and a concentrated tailings;

[0017] (3) The roughing tailings and the concentrating tailings are mixed, 0.2-0.4 kg / t of collector is added, and a scavenging is performed to obtain scavenging concentrate and scavenging tailings. The scavenging tailings are discarded, and the scavenging concentrate is returned to the roughing operation for closed-circuit flotation to finally obtain concentrate.

[0018] Furthermore, the regulator is sodium carbonate, the inhibitor is sulfonic acid-phosphoric acid double-modified cellulose, and the collector is a mixture of dodecylamine and sodium oleate, wherein the weight ratio of dodecylamine to sodium oleate is 3:1.

[0019] Furthermore, the preparation method of the sulfonic acid-phosphoric acid double-modified cellulose is:

[0020] The carboxymethyl cellulose is dispersed in deionized water, stirred for 20-40 minutes, and aminosulfonic acid is added. The pH value is adjusted to 5-6 with a 5% sodium hydroxide solution by mass, and the mixture is reacted in a water bath at 60-100° C. for 2-5 hours. The mixture is cooled to room temperature, precipitated and washed with ethanol, and vacuum dried at 50-70° C. to obtain sulfonated carboxymethyl cellulose. The sulfonated carboxymethyl cellulose is mixed with deionized water, sodium tripolyphosphate and urea are added, and the pH value is adjusted to 9-10 with a 5% sodium hydroxide solution by mass, and the mixture is reacted at 70-90° C. for 3-5 hours. The reaction solution is adjusted to a pH value of 7-7.5 with hydrochloric acid, precipitated and washed with ethanol, and dried to obtain sulfonic acid-phosphoric acid double-modified cellulose.

[0021] Furthermore, the usage ratio of the carboxymethyl cellulose, deionized water and aminosulfonic acid is 8-15g:120-180mL:2-5g; the usage ratio of the sulfonated carboxymethyl cellulose, deionized water, sodium tripolyphosphate and urea is 8-15g:80-150mL:1-5g:0.5-1.0g.

[0022] Furthermore, in step S3, the filter press is performed using a plate and frame filter press with a pressure set to 0.8-1.2 MPa, and the moisture content of the obtained filter cake is ≤18%; the drying is performed in a rotary drying kiln with a temperature controlled at 200-250°C for 1-2 hours, and the outlet moisture is ≤1%.

[0023] Furthermore, the gradient sintering method in step S4 is:

[0024] Stage 1: room temperature - 600°C, heating rate 2°C / min;

[0025] Stage 2: 600°C-1450°C, heating rate 5°C / min;

[0026] Stage 3: 1450℃-1600℃, heating rate is 2℃ / min.

[0027] An iron-containing corundum-high iron mullite solid solution raw material comprises the following components by weight percentage: 5-30wt% silicon dioxide, 5-12wt% iron oxide, 1-3wt% titanium dioxide, 1-3wt% calcium oxide, 0.1-1wt% other impurities, and the balance being aluminum oxide.

[0028] Beneficial effects of the present invention:

[0029] (1) Phosphate groups of sulfonic acid-phosphoric acid double-modified cellulose (-PO4 2-) specifically binds to Al-OH in bauxite to form a stable Al-OP bond, effectively inhibiting the excessive floating of aluminum minerals, while Fe2O3 minerals are not affected due to differences in surface properties. The Al2O3 recovery rate is improved, and the Fe2O3 retention rate is increased, ensuring a stable iron-aluminum ratio in subsequent sintering. In addition, the sulfonic acid-phosphoric acid double-modified cellulose has a weak inhibition on silicate minerals. When combined with a collector, it can effectively desiliconize and avoid the formation of excessive glass phase during sintering that affects high-temperature performance. The sulfonic acid-phosphoric acid double-modified cellulose inhibitor can accurately control the Al / Si / Fe ratio to achieve raw material homogenization and composition optimization.

[0030] (2) Sulfonic acid group (-SO3H) has a synergistic effect, which can enhance the water solubility and dispersibility of sulfonic acid-phosphoric acid double-modified cellulose, avoid the agglomeration of the reagent, make the inhibitor evenly cover the surface of the aluminum mineral, and reduce the dosage of the reagent;

[0031] (3) The microscopic distribution of Fe2O3 and Al2O3 in the flotation concentrate is more uniform, and Fe 3+ It is easier to diffuse into the corundum lattice to form a homogeneous solid solution, inhibit the aggregation of free Fe2O3, and the evenly distributed Fe2O3 reduces the Fe2O3→Fe3O4 reduction reaction caused by local enrichment, avoids the formation of low-melting-point phases, improves the refractoriness of the material, and realizes the efficient conversion of low-grade bauxite to prepare high-performance refractory materials, thereby improving both resource utilization and product added value. DETAILED DESCRIPTION

[0032] The following is a clear and complete description of the technical solutions in the embodiments of the present invention. Obviously, the embodiments described are only some embodiments of the present invention, not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making any creative efforts are within the scope of protection of the present invention.

[0033] The gradient sintering method in the following examples is:

[0034] Stage 1: room temperature - 600°C, heating rate 2°C / min;

[0035] Stage 2: 600°C-1450°C, heating rate 5°C / min;

[0036] Stage 3: 1450℃-1600℃, heating rate is 2℃ / min.

[0037] Example 1

[0038] A method for preparing an iron-containing corundum-high-iron mullite solid solution raw material comprises the following steps:

[0039] S1. Low-grade bauxite (aluminum-silicon ratio of 1.5:1; alumina content of 40%, main mineral phase diaspore) is selected as raw material, the raw material is coarsely crushed to a particle size of ≤50 mm using a jaw crusher, then finely crushed to a particle size of ≤2 mm using a hammer crusher, and passed through a 100-mesh sieve to obtain pretreated particles;

[0040] S2. The pretreated particles are mixed and piled, and homogenized for 2 days using a flat-laying and straight-taking method to obtain homogenized ore particles;

[0041] S3. The homogenized ore particles are subjected to a flotation process. The concentrate obtained by flotation is filtered (using a plate and frame filter press with a pressure set at 0.8 MPa, and the moisture content of the filter cake is ≤18%), and dried (in a rotary drying kiln at a temperature controlled at 200° C. for 1 hour, and the outlet moisture content is ≤1%) to obtain concentrate particles;

[0042] S4. Add 3% sodium lignin sulfonate by mass to the concentrate particles, press them into cylindrical bodies with a hydraulic press, perform gradient sintering on the cylindrical bodies, keep them warm for 4 hours, cool them to 200°C and then take them out of the furnace to obtain a bulk density of 2.4 g / cm 3 The iron-containing corundum-high iron mullite solid solution raw material includes the following components by weight percentage: 18.2wt% of silicon dioxide, 5wt% of iron oxide, 1wt% of titanium dioxide, 1wt% of calcium oxide, 0.1wt% of other impurities, and the balance is aluminum oxide.

[0043] The flotation process in step S3 is:

[0044] (1) Grinding the homogenized ore particles to obtain a mineral powder material with a particle size of ≤0.075 mm, concentrating the mineral powder material to obtain a concentrated ore pulp with a mass concentration of 30%, and sequentially adding 2 kg / t of sodium carbonate, 0.5 kg / t of sulfonic acid-phosphoric acid double-modified cellulose, 0.8 kg / t of dodecylamine and sodium oleate (the weight ratio of dodecylamine to sodium oleate is 3:1), and performing a roughing process to obtain a roughing concentrate and a roughing tailing;

[0045] (2) Adding 0.1 kg / t of sulfonic acid-phosphoric acid double-modified cellulose and 0.05 kg / t of dodecylamine and sodium oleate (the weight ratio of dodecylamine to sodium oleate is 3:1) to the rougher concentrate, maintaining the pH at 9.0, and performing a primary concentration to obtain a concentrated concentrate and a concentrated tailings;

[0046] (3) The roughing tailings and the beneficiated tailings are mixed, and 0.2 kg / t of dodecylamine and sodium oleate (the weight ratio of dodecylamine to sodium oleate is 3:1) are added to perform a scavenging operation to obtain scavenged concentrate and scavenged tailings. The scavenged tailings are discarded, and the scavenged concentrate is returned to the roughing operation for closed-circuit flotation (roughing once, beneficiation once, and scavenging once) to finally obtain the concentrate.

[0047] The preparation method of the sulfonic acid-phosphoric acid double-modified cellulose is:

[0048] 8.0 g of carboxymethyl cellulose was dispersed in 120 mL of deionized water, stirred for 20 min, 2.0 g of aminosulfonic acid was added, the pH was adjusted to 5.0 with a 5% sodium hydroxide solution, the reaction was carried out in a water bath at 60° C. for 2 h, the mixture was cooled to room temperature, precipitated and washed with ethanol, and dried in a vacuum at 50° C. to obtain sulfonated carboxymethyl cellulose; 8.0 g of sulfonated carboxymethyl cellulose was mixed with 80 mL of deionized water, 1.0 g of sodium tripolyphosphate and 0.5 g of urea were added, the pH was adjusted to 9.0 with a 5% sodium hydroxide solution, the reaction was carried out at 70° C. for 3 h, the pH of the reaction solution was adjusted to 7.0 with hydrochloric acid, the mixture was precipitated and washed with ethanol, and dried to obtain sulfonic acid-phosphoric acid double-modified cellulose.

[0049] Example 2

[0050] A method for preparing an iron-containing corundum-high-iron mullite solid solution raw material comprises the following steps:

[0051] S1. Low-grade bauxite (aluminum-silicon ratio of 2.6:1; alumina content of 60%, main mineral phase diaspore) is selected as raw material, the raw material is coarsely crushed to a particle size of ≤50 mm using a jaw crusher, then finely crushed to a particle size of ≤2 mm using a hammer crusher, and passed through a 100-mesh sieve to obtain pretreated particles;

[0052] S2. The pretreated particles are mixed and piled, and homogenized for 3 days using a flat-laying and straight-taking method to obtain homogenized ore particles;

[0053] S3. The homogenized ore particles are subjected to a flotation process. The concentrate obtained by flotation is filtered (using a plate and frame filter press with a pressure set at 1.2 MPa, and the moisture content of the filter cake is ≤18%), and dried (in a rotary drying kiln at a temperature controlled at 250° C. for 1 hour, and the outlet moisture content is ≤1%) to obtain concentrate particles;

[0054] S4. Add 5% sodium lignin sulfonate by mass to the concentrate particles, press them into cylindrical bodies with a hydraulic press, perform gradient sintering on the cylindrical bodies, keep them warm for 6 hours, cool them to 400℃ and then take them out of the furnace to obtain a bulk density of 3.2g / cm 3 The iron-containing corundum-high iron mullite solid solution raw material includes the following components by weight percentage: 15wt% silicon dioxide, 12wt% iron oxide, 3wt% titanium dioxide, 3wt% calcium oxide, 1wt% other impurities, and the balance is aluminum oxide.

[0055] The flotation process in step S3 is:

[0056] (1) Grinding the homogenized ore particles to obtain a mineral powder material with a particle size of ≤0.075 mm, concentrating the mineral powder material to obtain a concentrated ore pulp with a mass concentration of 50%, and sequentially adding 3 kg / t of sodium carbonate, 1.2 kg / t of sulfonic acid-phosphoric acid double-modified cellulose, 1.5 kg / t of dodecylamine and sodium oleate (the weight ratio of dodecylamine to sodium oleate is 3:1), and performing a roughing process to obtain a roughing concentrate and a roughing tailing;

[0057] (2) Adding 0.3 kg / t of sulfonic acid-phosphoric acid double-modified cellulose and 0.1 kg / t of dodecylamine and sodium oleate (the weight ratio of dodecylamine to sodium oleate is 3:1) to the rougher concentrate, maintaining the pH at 9.5, and performing a primary concentration to obtain a concentrated concentrate and a concentrated tailings;

[0058] (3) The roughing tailings and the beneficiated tailings are mixed, and 0.4 kg / t of dodecylamine and sodium oleate (the weight ratio of dodecylamine to sodium oleate is 3:1) are added. A scavenging is performed to obtain scavenged concentrate and scavenged tailings. The scavenged tailings are discarded, and the scavenged concentrate is returned to the roughing operation for closed-circuit flotation (roughing once, beneficiation once, and scavenging twice) to finally obtain the concentrate.

[0059] The preparation method of the sulfonic acid-phosphoric acid double-modified cellulose is:

[0060] 15.0 g of carboxymethyl cellulose was dispersed in 180 mL of deionized water, stirred for 40 min, 5.0 g of aminosulfonic acid was added, the pH was adjusted to 6.0 with a 5% sodium hydroxide solution, the reaction was carried out in a water bath at 100° C. for 5 h, the mixture was cooled to room temperature, precipitated and washed with ethanol, and dried in a vacuum at 70° C. to obtain sulfonated carboxymethyl cellulose; 15.0 g of sulfonated carboxymethyl cellulose was mixed with 150 mL of deionized water, 5.0 g of sodium tripolyphosphate and 1.0 g of urea were added, the pH was adjusted to 10.0 with a 5% sodium hydroxide solution, the reaction was carried out at 90° C. for 5 h, the pH of the reaction solution was adjusted to 7.5 with hydrochloric acid, the mixture was precipitated and washed with ethanol, and dried to obtain sulfonic acid-phosphoric acid double-modified cellulose.

[0061] Example 3

[0062] A method for preparing an iron-containing corundum-high-iron mullite solid solution raw material comprises the following steps:

[0063] S1. Low-grade bauxite (aluminum-silicon ratio of 2.1:1; alumina content of 50%, main mineral phase diaspore) is selected as raw material, the raw material is coarsely crushed to a particle size of ≤50 mm using a jaw crusher, and then finely crushed to a particle size of ≤2 mm using a hammer crusher, and passed through a 100-mesh sieve to obtain pretreated particles;

[0064] S2. The pretreated particles are mixed and piled, and homogenized for 2.5 days using a flat-laying and straight-taking method to obtain homogenized ore particles;

[0065] S3. The homogenized ore particles are subjected to a flotation process. The concentrate obtained by flotation is filtered (using a plate and frame filter press with a pressure set at 1.0 MPa, and the moisture content of the filter cake is ≤18%), and dried (in a rotary drying kiln at a temperature controlled at 225° C. for 1.5 hours, and the outlet moisture content is ≤1%) to obtain concentrate particles;

[0066] S4. Add 4% sodium lignin sulfonate by mass to the concentrate particles, press them into cylindrical bodies with a hydraulic press, perform gradient sintering on the cylindrical bodies, keep them warm for 5 hours, cool them to 300°C and then take them out of the furnace to obtain a bulk density of 2.8 g / cm 3 The iron-containing corundum-high iron mullite solid solution raw material includes the following components by weight percentage: 16.4wt% of silicon dioxide, 8.5wt% of iron oxide, 2wt% of titanium dioxide, 2wt% of calcium oxide, 0.55wt% of other impurities, and the balance is aluminum oxide.

[0067] The flotation process in step S3 is:

[0068] (1) Grinding the homogenized ore particles to obtain a mineral powder material with a particle size of ≤0.075 mm, concentrating the mineral powder material to obtain a concentrated ore pulp with a mass concentration of 40%, and sequentially adding 2.5 kg / t of sodium carbonate, 0.85 kg / t of sulfonic acid-phosphoric acid double-modified cellulose, 1.15 kg / t of dodecylamine and sodium oleate (the weight ratio of dodecylamine to sodium oleate is 3:1), and performing a roughing process to obtain a roughing concentrate and a roughing tailing;

[0069] (2) Adding 0.2 kg / t of sulfonic acid-phosphoric acid double-modified cellulose and 0.07 kg / t of dodecylamine and sodium oleate (the weight ratio of dodecylamine to sodium oleate is 3:1) to the rougher concentrate, maintaining the pH at 9.2, and performing a primary concentration to obtain a concentrated concentrate and a concentrated tailings;

[0070] (3) The roughing tailings and the beneficiated tailings are mixed, and 0.3 kg / t of dodecylamine and sodium oleate (the weight ratio of dodecylamine to sodium oleate is 3:1) are added to perform a scavenging operation to obtain scavenged concentrate and scavenged tailings. The scavenged tailings are discarded, and the scavenged concentrate is returned to the roughing operation for closed-circuit flotation (roughing once, beneficiation once, and scavenging once) to finally obtain the concentrate.

[0071] The preparation method of the sulfonic acid-phosphoric acid double-modified cellulose is:

[0072] 11.0 g of carboxymethyl cellulose was dispersed in 150 mL of deionized water, stirred for 30 min, 3.5 g of aminosulfonic acid was added, the pH was adjusted to 5.5 with a 5% sodium hydroxide solution, the reaction was carried out in a water bath at 80° C. for 3.5 h, cooled to room temperature, precipitated and washed with ethanol, and dried in a vacuum at 60° C. to obtain sulfonated carboxymethyl cellulose; 11.0 g of sulfonated carboxymethyl cellulose was mixed with 115 mL of deionized water, 3.0 g of sodium tripolyphosphate and 0.75 g of urea were added, the pH was adjusted to 9.5 with a 5% sodium hydroxide solution, the reaction was carried out at 80° C. for 4 h, the reaction solution was adjusted to pH 7.2 with hydrochloric acid, precipitated and washed with ethanol, and dried to obtain sulfonic acid-phosphoric acid double-modified cellulose.

[0073] Example 4

[0074] A method for preparing an iron-containing corundum-high-iron mullite solid solution raw material comprises the following steps:

[0075] S1. Low-grade bauxite (aluminum-silicon ratio of 1.9:1; alumina content of 56%, main mineral phase diaspore) is selected as raw material, the raw material is coarsely crushed to a particle size of ≤50 mm using a jaw crusher, then finely crushed to a particle size of ≤2 mm using a hammer crusher, and passed through a 100-mesh sieve to obtain pretreated particles;

[0076] S2. The pretreated particles are mixed and piled, and homogenized for 3 days using a flat-laying and straight-taking method to obtain homogenized ore particles;

[0077] S3. The homogenized ore particles are subjected to a flotation process. The concentrate obtained by flotation is filtered (using a plate and frame filter press with a pressure set at 1.0 MPa, and the moisture content of the filter cake is ≤18%), and dried (in a rotary drying kiln at a temperature controlled at 200° C. for 1 hour, and the outlet moisture content is ≤1%) to obtain concentrate particles;

[0078] S4. Add 5% sodium lignin sulfonate by mass to the concentrate particles, press them into cylindrical bodies with a hydraulic press, perform gradient sintering on the cylindrical bodies, keep them warm for 5 hours, cool them to 300°C and then take them out of the furnace to obtain a bulk density of 2.9 g / cm 3 The iron-containing corundum-high iron mullite solid solution raw material includes the following components by weight percentage: 14.8wt% of silicon dioxide, 11.21wt% of iron oxide, 2.06wt% of titanium dioxide, 2.52wt% of calcium oxide, 0.1wt% of other impurities, and the balance is aluminum oxide.

[0079] The flotation process in step S3 is:

[0080] (1) Grinding the homogenized ore particles to obtain a mineral powder material with a particle size of ≤0.075 mm, concentrating the mineral powder material to obtain a concentrated ore pulp with a mass concentration of 30%, and sequentially adding 2.5 kg / t of sodium carbonate, 0.80 kg / t of sulfonic acid-phosphoric acid double-modified cellulose, 1.10 kg / t of dodecylamine and sodium oleate (the weight ratio of dodecylamine to sodium oleate is 3:1), and performing a roughing process to obtain a roughing concentrate and a roughing tailing;

[0081] (2) Adding 0.2 kg / t of sulfonic acid-phosphoric acid double-modified cellulose and 0.05 kg / t of dodecylamine and sodium oleate (the weight ratio of dodecylamine to sodium oleate is 3:1) to the rougher concentrate, maintaining the pH at 9.0, and performing a primary concentration to obtain a concentrated concentrate and a concentrated tailings;

[0082] (3) The roughing tailings and the beneficiated tailings are mixed, and 0.3 kg / t of dodecylamine and sodium oleate (the weight ratio of dodecylamine to sodium oleate is 3:1) are added to perform a scavenging operation to obtain scavenged concentrate and scavenged tailings. The scavenged tailings are discarded, and the scavenged concentrate is returned to the roughing operation for closed-circuit flotation (roughing once, beneficiation once, and scavenging once) to finally obtain the concentrate.

[0083] The preparation method of the sulfonic acid-phosphoric acid double-modified cellulose is:

[0084] 10.0 g of carboxymethyl cellulose was dispersed in 150 mL of deionized water, stirred for 30 min, 3.2 g of aminosulfonic acid was added, the pH was adjusted to 5.5 with a 5% sodium hydroxide solution, the reaction was carried out in a water bath at 80°C for 3 h, cooled to room temperature, precipitated and washed with ethanol, and dried in a vacuum at 60°C to obtain sulfonated carboxymethyl cellulose; 10.0 g of sulfonated carboxymethyl cellulose was mixed with 100 mL of deionized water, 2.1 g of sodium tripolyphosphate and 0.5 g of urea were added, the pH was adjusted to 9.5 with a 5% sodium hydroxide solution, the reaction was carried out at 85°C for 4 h, the pH of the reaction solution was adjusted to 7.0 with hydrochloric acid, precipitated and washed with ethanol, and dried to obtain sulfonic acid-phosphoric acid double-modified cellulose.

[0085] Example 5

[0086] A method for preparing an iron-containing corundum-high-iron mullite solid solution raw material comprises the following steps:

[0087] S1. Low-grade bauxite (aluminum-silicon ratio of 1.9:1; alumina content of 56%, main mineral phase diaspore) is selected as raw material, the raw material is coarsely crushed to a particle size of ≤50 mm using a jaw crusher, then finely crushed to a particle size of ≤2 mm using a hammer crusher, and passed through a 100-mesh sieve to obtain pretreated particles;

[0088] S2. The pretreated particles are mixed and piled, and homogenized for 3 days using a flat-laying and straight-taking method to obtain homogenized ore particles;

[0089] S3. The homogenized ore particles are subjected to a flotation process. The concentrate obtained by flotation is filtered (using a plate and frame filter press with a pressure set at 1.0 MPa, and the moisture content of the filter cake is ≤18%), and dried (in a rotary drying kiln at a temperature controlled at 200° C. for 1 hour, and the outlet moisture content is ≤1%) to obtain concentrate particles;

[0090] S4. Add 5% sodium lignin sulfonate by mass to the concentrate particles, press them into cylindrical bodies with a hydraulic press, perform gradient sintering on the cylindrical bodies, keep them warm for 5 hours, cool them to 300°C and then take them out of the furnace to obtain a bulk density of 3.0 g / cm 3 The iron-containing corundum-high iron mullite solid solution raw material includes the following components by weight percentage: 15.8wt% of silicon dioxide, 9.24wt% of iron oxide, 2.18wt% of titanium dioxide, 1.73wt% of calcium oxide, 0.1wt% of other impurities, and the balance is aluminum oxide.

[0091] The flotation process in step S3 is:

[0092] (1) Grinding the homogenized ore particles to obtain a mineral powder material with a particle size of ≤0.075 mm, concentrating the mineral powder material to obtain a concentrated ore pulp with a mass concentration of 30%, and sequentially adding 2.5 kg / t of sodium carbonate, 0.80 kg / t of sulfonic acid-phosphoric acid double-modified cellulose, 1.10 kg / t of dodecylamine and sodium oleate (the weight ratio of dodecylamine to sodium oleate is 3:1), and performing a roughing process to obtain a roughing concentrate and a roughing tailing;

[0093] (2) Adding 0.2 kg / t of sulfonic acid-phosphoric acid double-modified cellulose and 0.05 kg / t of dodecylamine and sodium oleate (the weight ratio of dodecylamine to sodium oleate is 3:1) to the rougher concentrate, maintaining the pH at 9.0, and performing a primary concentration to obtain a concentrated concentrate and a concentrated tailings;

[0094] (3) The roughing tailings and the beneficiated tailings are mixed, and 0.3 kg / t of dodecylamine and sodium oleate (the weight ratio of dodecylamine to sodium oleate is 3:1) are added to perform a scavenging operation to obtain scavenged concentrate and scavenged tailings. The scavenged tailings are discarded, and the scavenged concentrate is returned to the roughing operation for closed-circuit flotation (roughing once, beneficiation once, and scavenging twice) to finally obtain the concentrate.

[0095] The preparation method of the sulfonic acid-phosphoric acid double-modified cellulose is:

[0096] 10.0 g of carboxymethyl cellulose was dispersed in 150 mL of deionized water, stirred for 30 min, 3.2 g of aminosulfonic acid was added, the pH was adjusted to 5.5 with a 5% sodium hydroxide solution, the reaction was carried out in a water bath at 80°C for 3 h, cooled to room temperature, precipitated and washed with ethanol, and dried in a vacuum at 60°C to obtain sulfonated carboxymethyl cellulose; 10.0 g of sulfonated carboxymethyl cellulose was mixed with 100 mL of deionized water, 2.1 g of sodium tripolyphosphate and 0.5 g of urea were added, the pH was adjusted to 9.5 with a 5% sodium hydroxide solution, the reaction was carried out at 85°C for 4 h, the pH of the reaction solution was adjusted to 7.0 with hydrochloric acid, precipitated and washed with ethanol, and dried to obtain sulfonic acid-phosphoric acid double-modified cellulose.

[0097] Comparative Example 1

[0098] A method for preparing an iron-containing corundum-high-iron mullite solid solution raw material comprises the following steps:

[0099] S1. Low-grade bauxite (aluminum-silicon ratio of 1.9:1; alumina content of 56%, main mineral phase diaspore) is selected as raw material, the raw material is coarsely crushed to a particle size of ≤50 mm using a jaw crusher, then finely crushed to a particle size of ≤2 mm using a hammer crusher, and passed through a 100-mesh sieve to obtain pretreated particles;

[0100] S2. The pretreated particles are mixed and piled, and homogenized for 3 days using a flat-laying and straight-taking method to obtain homogenized ore particles;

[0101] S3. The homogenized ore particles are subjected to a flotation process. The concentrate obtained by flotation is filtered (using a plate and frame filter press with a pressure set at 1.0 MPa, and the moisture content of the filter cake is ≤18%), and dried (in a rotary drying kiln at a temperature controlled at 200° C. for 1 hour, and the outlet moisture content is ≤1%) to obtain concentrate particles;

[0102] S4. Add 5% sodium lignin sulfonate by mass to the concentrate particles, press them into cylindrical bodies with a hydraulic press, perform gradient sintering on the cylindrical bodies, keep them warm for 5 hours, cool them to 300°C and then take them out of the furnace to obtain a bulk density of 2.43 g / cm 3 The iron-containing corundum-high iron mullite solid solution raw material includes the following components by weight percentage: 29.7wt% of silicon dioxide, 6.5wt% of iron oxide, 2.11wt% of titanium dioxide, 2.03wt% of calcium oxide, 0.15wt% of other impurities, and the balance is aluminum oxide.

[0103] The flotation process in step S3 is:

[0104] (1) Grinding the homogenized ore particles to obtain a mineral powder material with a particle size of ≤0.075 mm, concentrating the mineral powder material to obtain a concentrated ore pulp with a mass concentration of 30%, and sequentially adding 2.5 kg / t of sodium carbonate, 0.80 kg / t of carboxymethyl cellulose, 1.10 kg / t of dodecylamine and sodium oleate (the weight ratio of dodecylamine to sodium oleate is 3:1), and performing a roughing process to obtain a roughing concentrate and a roughing tailing;

[0105] (2) Adding 0.2 kg / t of carboxymethyl cellulose and 0.05 kg / t of dodecylamine and sodium oleate (the weight ratio of dodecylamine to sodium oleate is 3:1) to the rougher concentrate, maintaining the pH at 9.0, and performing a primary concentration to obtain a concentrated concentrate and a concentrated tailings;

[0106] (3) The roughing tailings and the beneficiated tailings are mixed, and 0.3 kg / t of dodecylamine and sodium oleate (the weight ratio of dodecylamine to sodium oleate is 3:1) are added to perform a scavenging operation to obtain scavenged concentrate and scavenged tailings. The scavenged tailings are discarded, and the scavenged concentrate is returned to the roughing operation for closed-circuit flotation (roughing once, beneficiation once, and scavenging once) to finally obtain the concentrate.

[0107] Comparative Example 2

[0108] A method for preparing an iron-containing corundum-high-iron mullite solid solution raw material comprises the following steps:

[0109] S1. Low-grade bauxite (aluminum-silicon ratio of 1.9:1; alumina content of 56%, main mineral phase diaspore) is selected as raw material, the raw material is coarsely crushed to a particle size of ≤50 mm using a jaw crusher, then finely crushed to a particle size of ≤2 mm using a hammer crusher, and passed through a 100-mesh sieve to obtain pretreated particles;

[0110] S2. The pretreated particles are mixed and piled, and homogenized for 3 days using a flat-laying and straight-taking method to obtain homogenized ore particles;

[0111] S3. The homogenized ore particles are subjected to a flotation process. The concentrate obtained by flotation is filtered (using a plate and frame filter press with a pressure set at 1.0 MPa, and the moisture content of the filter cake is ≤18%), and dried (in a rotary drying kiln at a temperature controlled at 200° C. for 1 hour, and the outlet moisture content is ≤1%) to obtain concentrate particles;

[0112] S4. Add 5% sodium lignin sulfonate by mass to the concentrate particles, press them into cylindrical bodies with a hydraulic press, perform gradient sintering on the cylindrical bodies, keep them warm for 5 hours, cool them to 300°C and then take them out of the furnace to obtain a bulk density of 2.52 g / cm 3The iron-containing corundum-high iron mullite solid solution raw material includes the following components by weight percentage: 27.6wt% of silicon dioxide, 7.0wt% of iron oxide, 2.08wt% of titanium dioxide, 2.31wt% of calcium oxide, 0.14wt% of other impurities, and the balance is aluminum oxide.

[0113] The flotation process in step S3 is:

[0114] (1) Grinding the homogenized ore particles to obtain a mineral powder material with a particle size of ≤0.075 mm, concentrating the mineral powder material to obtain a concentrated ore pulp with a mass concentration of 30%, sequentially adding 2.5 kg / t of sodium carbonate, 0.80 kg / t of sulfonated carboxymethyl cellulose, 1.10 kg / t of dodecylamine and sodium oleate (the weight ratio of dodecylamine to sodium oleate is 3:1), and performing a roughing process to obtain a roughing concentrate and a roughing tailing;

[0115] (2) adding 0.2 kg / t of sulfonated carboxymethyl cellulose and 0.05 kg / t of dodecylamine and sodium oleate (the weight ratio of dodecylamine to sodium oleate is 3:1) to the rougher concentrate, maintaining the pH at 9.0, and performing a primary concentration to obtain a concentrated concentrate and a concentrated tailing;

[0116] (3) The roughing tailings and the beneficiated tailings are mixed, and 0.3 kg / t of dodecylamine and sodium oleate (the weight ratio of dodecylamine to sodium oleate is 3:1) are added to perform a scavenging operation to obtain scavenged concentrate and scavenged tailings. The scavenged tailings are discarded, and the scavenged concentrate is returned to the roughing operation for closed-circuit flotation (roughing once, beneficiation once, and scavenging once) to finally obtain the concentrate.

[0117] The preparation method of the sulfonated carboxymethyl cellulose is:

[0118] Disperse 10.0 g of carboxymethyl cellulose in 150 mL of deionized water, stir for 30 min, add 3.2 g of aminosulfonic acid, adjust the pH to 5.5 with 5% sodium hydroxide solution, react in a water bath at 80°C for 3 h, cool to room temperature, precipitate and wash with ethanol, and dry in vacuo at 60°C to obtain sulfonated carboxymethyl cellulose.

[0119] Comparative Example 3

[0120] A method for preparing an iron-containing corundum-high-iron mullite solid solution raw material comprises the following steps:

[0121] S1. Low-grade bauxite (aluminum-silicon ratio of 1.9:1; alumina content of 56%, main mineral phase diaspore) is selected as raw material, the raw material is coarsely crushed to a particle size of ≤50 mm using a jaw crusher, then finely crushed to a particle size of ≤2 mm using a hammer crusher, and passed through a 100-mesh sieve to obtain pretreated particles;

[0122] S2. The pretreated particles are mixed and piled, and homogenized for 3 days using a flat-laying and straight-taking method to obtain homogenized ore particles;

[0123] S3. The homogenized ore particles are subjected to a flotation process. The concentrate obtained by flotation is filtered (using a plate and frame filter press with a pressure set at 1.0 MPa, and the moisture content of the filter cake is ≤18%), and dried (in a rotary drying kiln at a temperature controlled at 200° C. for 1 hour, and the outlet moisture content is ≤1%) to obtain concentrate particles;

[0124] S4. Add 5% sodium lignin sulfonate by mass to the concentrate particles, press them into cylindrical bodies with a hydraulic press, perform gradient sintering on the cylindrical bodies, keep them warm for 5 hours, cool them to 300°C and then take them out of the furnace to obtain a bulk density of 2.63 g / cm 3 The iron-containing corundum-high iron mullite solid solution raw material includes the following components by weight percentage: 25.9wt% of silicon dioxide, 7.3wt% of iron oxide, 2.54wt% of titanium dioxide, 2.07wt% of calcium oxide, 0.18wt% of other impurities, and the balance is aluminum oxide.

[0125] The flotation process in step S3 is:

[0126] (1) Grinding the homogenized ore particles to obtain a mineral powder material with a particle size of ≤0.075 mm, concentrating the mineral powder material to obtain a concentrated ore pulp with a mass concentration of 30%, and sequentially adding 2.5 kg / t of sodium carbonate, 0.80 kg / t of phosphated carboxymethyl cellulose, 1.10 kg / t of dodecylamine and sodium oleate (the weight ratio of dodecylamine to sodium oleate is 3:1), and performing a roughing process to obtain a roughing concentrate and a roughing tailing;

[0127] (2) Adding 0.2 kg / t of phosphated carboxymethyl cellulose and 0.05 kg / t of dodecylamine and sodium oleate (the weight ratio of dodecylamine to sodium oleate is 3:1) to the rougher concentrate, maintaining the pH at 9.0, and performing a primary concentration to obtain a concentrated concentrate and a concentrated tailings;

[0128] (3) The roughing tailings and the beneficiated tailings are mixed, and 0.3 kg / t of dodecylamine and sodium oleate (the weight ratio of dodecylamine to sodium oleate is 3:1) are added to perform a scavenging operation to obtain scavenged concentrate and scavenged tailings. The scavenged tailings are discarded, and the scavenged concentrate is returned to the roughing operation for closed-circuit flotation (roughing once, beneficiation once, and scavenging once) to finally obtain the concentrate.

[0129] The preparation method of the phosphated carboxymethyl cellulose is:

[0130] Mix 10.0 g of carboxymethyl cellulose with 100 mL of deionized water, add 2.1 g of sodium tripolyphosphate and 0.5 g of urea, adjust the pH to 9.5 with a 5% mass fraction of sodium hydroxide solution, react at 85°C for 4 h, adjust the pH of the reaction solution to 7.0 with hydrochloric acid, precipitate and wash with ethanol, and dry to obtain phosphated carboxymethyl cellulose.

[0131] Comparative Example 4

[0132] A method for preparing an iron-containing corundum-high-iron mullite solid solution raw material comprises the following steps:

[0133] S1. Low-grade bauxite (aluminum-silicon ratio of 1.9:1; alumina content of 56%, main mineral phase diaspore) is selected as raw material, the raw material is coarsely crushed to a particle size of ≤50 mm using a jaw crusher, then finely crushed to a particle size of ≤2 mm using a hammer crusher, and passed through a 100-mesh sieve to obtain pretreated particles;

[0134] S2. The pretreated particles are mixed and piled, and homogenized for 3 days using a flat-laying and straight-taking method to obtain homogenized ore particles;

[0135] S3. The homogenized ore particles are subjected to a flotation process. The concentrate obtained by flotation is filtered (using a plate and frame filter press with a pressure set at 1.0 MPa, and the moisture content of the filter cake is ≤18%), and dried (in a rotary drying kiln at a temperature controlled at 200° C. for 1 hour, and the outlet moisture content is ≤1%) to obtain concentrate particles;

[0136] S4. Add 5% sodium lignin sulfonate by mass to the concentrate particles, press them into cylindrical bodies with a hydraulic press, perform gradient sintering on the cylindrical bodies, keep them warm for 5 hours, cool them to 300°C and then take them out of the furnace to obtain a bulk density of 2.9 g / cm 3 The iron-containing corundum-high iron mullite solid solution raw material includes the following components by weight percentage: 22.8wt% of silicon dioxide, 7.5wt% of iron oxide, 1.86wt% of titanium dioxide, 1.52wt% of calcium oxide, 0.13wt% of other impurities, and the balance is aluminum oxide.

[0137] The flotation process in step S3 is:

[0138] (1) Grinding the homogenized ore particles to obtain a mineral powder material with a particle size of ≤0.075 mm, concentrating the mineral powder material to obtain a concentrated ore pulp with a mass concentration of 30%, sequentially adding 2.5 kg / t of sodium carbonate, 0.80 kg / t of sulfonic acid-phosphoric acid double-modified cellulose, and 1.10 kg / t of dodecylamine, and performing a roughing operation to obtain a roughing concentrate and a roughing tailing;

[0139] (2) adding 0.2 kg / t of sulfonic acid-phosphoric acid double-modified cellulose and 0.05 kg / t of dodecylamine to the rougher concentrate, maintaining the pH at 9.0, and performing a primary concentration to obtain a concentrated concentrate and a concentrated tailing;

[0140] (3) The roughing tailings and the beneficiated tailings are mixed, 0.3 kg / t of dodecylamine is added, and a scavenging is performed to obtain a scavenged concentrate and scavenged tailings. The scavenged tailings are discarded, and the scavenged concentrate is returned to the roughing operation for closed-circuit flotation (roughing once, beneficiation once, and scavenging once) to finally obtain a concentrate.

[0141] The preparation method of the sulfonic acid-phosphoric acid double-modified cellulose is:

[0142] 10.0 g of carboxymethyl cellulose was dispersed in 150 mL of deionized water, stirred for 30 min, 3.2 g of aminosulfonic acid was added, the pH was adjusted to 5.5 with a 5% sodium hydroxide solution, the reaction was carried out in a water bath at 80°C for 3 h, cooled to room temperature, precipitated and washed with ethanol, and dried in a vacuum at 60°C to obtain sulfonated carboxymethyl cellulose; 10.0 g of sulfonated carboxymethyl cellulose was mixed with 100 mL of deionized water, 2.1 g of sodium tripolyphosphate and 0.5 g of urea were added, the pH was adjusted to 9.5 with a 5% sodium hydroxide solution, the reaction was carried out at 85°C for 4 h, the pH of the reaction solution was adjusted to 7.0 with hydrochloric acid, precipitated and washed with ethanol, and dried to obtain sulfonic acid-phosphoric acid double-modified cellulose.

[0143] Comparative Example 5

[0144] A method for preparing an iron-containing corundum-high-iron mullite solid solution raw material comprises the following steps:

[0145] S1. Low-grade bauxite (aluminum-silicon ratio of 1.9:1; alumina content of 56%, main mineral phase diaspore) is selected as raw material, the raw material is coarsely crushed to a particle size of ≤50 mm using a jaw crusher, then finely crushed to a particle size of ≤2 mm using a hammer crusher, and passed through a 100-mesh sieve to obtain pretreated particles;

[0146] S2. The pretreated particles are mixed and piled, and homogenized for 3 days using a flat-laying and straight-taking method to obtain homogenized ore particles;

[0147] S3. The homogenized ore particles are subjected to a flotation process. The concentrate obtained by flotation is filtered (using a plate and frame filter press with a pressure set at 1.0 MPa, and the moisture content of the filter cake is ≤18%), and dried (in a rotary drying kiln at a temperature controlled at 200° C. for 1 hour, and the outlet moisture content is ≤1%) to obtain concentrate particles;

[0148] S4. Add 5% sodium lignin sulfonate by mass to the concentrate particles, press them into cylindrical bodies with a hydraulic press, perform gradient sintering on the cylindrical bodies, keep them warm for 5 hours, cool them to 300°C and then take them out of the furnace to obtain a bulk density of 2.9 g / cm 3 The iron-containing corundum-high iron mullite solid solution raw material includes the following components by weight percentage: 21.4wt% of silicon dioxide, 7.7wt% of iron oxide, 2.36wt% of titanium dioxide, 2.12wt% of calcium oxide, 0.17wt% of other impurities, and the balance is aluminum oxide.

[0149] The flotation process in step S3 is:

[0150] (1) Grinding the homogenized ore particles to obtain a mineral powder material with a particle size of ≤0.075 mm, concentrating the mineral powder material to obtain a concentrated ore pulp with a mass concentration of 30%, and sequentially adding 2.5 kg / t of sodium carbonate, 0.80 kg / t of sulfonic acid-phosphoric acid double-modified cellulose, and 1.10 kg / t of sodium oleate to perform a roughing operation to obtain a roughing concentrate and a roughing tailing;

[0151] (2) adding 0.2 kg / t of sulfonic acid-phosphoric acid double-modified cellulose and 0.05 kg / t of sodium oleate to the rougher concentrate, maintaining the pH at 9.0, and performing a primary concentration to obtain a concentrated concentrate and a concentrated tailing;

[0152] (3) The roughing tailings and the beneficiated tailings are mixed, 0.3 kg / t of sodium oleate is added, and a scavenging is performed to obtain a scavenged concentrate and scavenged tailings. The scavenged tailings are discarded, and the scavenged concentrate is returned to the roughing operation for closed-circuit flotation (roughing once, beneficiation once, and scavenging once) to finally obtain a concentrate.

[0153] The preparation method of the sulfonic acid-phosphoric acid double-modified cellulose is:

[0154] 10.0 g of carboxymethyl cellulose was dispersed in 150 mL of deionized water, stirred for 30 min, 3.2 g of aminosulfonic acid was added, the pH was adjusted to 5.5 with a 5% sodium hydroxide solution, the reaction was carried out in a water bath at 80°C for 3 h, cooled to room temperature, precipitated and washed with ethanol, and dried in a vacuum at 60°C to obtain sulfonated carboxymethyl cellulose; 10.0 g of sulfonated carboxymethyl cellulose was mixed with 100 mL of deionized water, 2.1 g of sodium tripolyphosphate and 0.5 g of urea were added, the pH was adjusted to 9.5 with a 5% sodium hydroxide solution, the reaction was carried out at 85°C for 4 h, the pH of the reaction solution was adjusted to 7.0 with hydrochloric acid, precipitated and washed with ethanol, and dried to obtain sulfonic acid-phosphoric acid double-modified cellulose.

[0155] The following is a further test of the effects of an iron-containing corundum-high iron mullite solid solution raw material prepared by the present invention: flotation efficiency: Al2O3 recovery rate (%) and concentrate aluminum-silicon ratio (A / S); sintered body properties: after sintering the flotation concentrate compact, the properties of the resulting sintered body: high-temperature flexural strength (MPa) and Fe2O3 solid solution content (%); the test results are described below.

[0156] The results are recorded in Table 1;

[0157] Table 1: Test results

[0158]

[0159]

[0160] According to the data in Table 1, it can be seen from the comparison between the examples of the present invention and the comparative examples that the use of the sulfonic acid-phosphoric acid double-modified cellulose prepared by the present invention as a depressant in the flotation process can achieve high concentrate grade and high recovery rate, improve the aluminum-silicon ratio of the bauxite concentrate, reduce the generation of low-melting point silicate impurities in the subsequent sintering process, and achieve efficient conversion of low-grade bauxite to prepare high-performance refractory materials, thereby improving both resource utilization and product added value.

[0161] The above content is merely an example and explanation of the concept of the present invention. Those skilled in the art may make various modifications or additions to the described specific embodiments or replace them in a similar manner. As long as they do not deviate from the concept of the invention or exceed the scope defined by the claims, they should all fall within the scope of protection of the present invention.

Claims

1. A method for preparing an iron-containing corundum-high iron mullite solid solution raw material, characterized in that: The following steps are involved: S1. Select low-grade bauxite as raw material and crush the raw material to obtain pre-treated particles; S2. The pretreated particles are mixed and piled, and homogenized for 2-3 days using a flat-laying and straight-taking method to obtain homogenized ore particles; S3, performing a flotation process on the homogenized ore particles, and filtering and drying the concentrate obtained by flotation to obtain concentrate particles; S4. Add 3-5% by mass of lignin sulfonate to the concentrate particles, press them into a cylindrical body with a hydraulic press, perform gradient sintering on the cylindrical body, keep it warm for 4-6 hours, cool it to 200-400°C with the furnace, and then take it out of the furnace to obtain an iron-containing corundum-high iron mullite solid solution raw material.

2. The method for preparing an iron-containing corundum-high iron mullite solid solution raw material according to claim 1, characterized in that: The low-grade bauxite in step S1 has an aluminum-silicon ratio of 1.5-2.6:1, an aluminum oxide content of 40-60%, and a main mineral phase of diaspore.

3. The method for preparing an iron-containing corundum-high iron mullite solid solution raw material according to claim 1, characterized in that: The flotation process in step S3 includes: roughing 1-2 times, cleaning 1-2 times, and scavenging 1-2 times.

4. The method for preparing an iron-containing corundum-high iron mullite solid solution raw material according to claim 1, characterized in that: The flotation process in step S3 is: (1) Grinding the homogenized ore particles to obtain a mineral powder material with a particle size of ≤0.075 mm, concentrating the mineral powder material to obtain a concentrated ore pulp with a mass concentration of 30-50%, sequentially adding 2-3 kg / t of a regulator, 0.5-1.2 kg / t of a depressant, and 0.8-1.5 kg / t of a collector, and performing a roughing operation to obtain a roughing concentrate and a roughing tailing; (2) adding 0.1-0.3 kg / t of inhibitor and 0.05-0.1 kg / t of collector to the rougher concentrate, maintaining the pH at 9.0-9.5, and performing a primary concentration to obtain a concentrated concentrate and a concentrated tailings; (3) The roughing tailings and the concentrating tailings are mixed, 0.2-0.4 kg / t of collector is added, and a scavenging is performed to obtain scavenging concentrate and scavenging tailings. The scavenging tailings are discarded, and the scavenging concentrate is returned to the roughing operation for closed-circuit flotation to finally obtain concentrate.

5. The method for preparing an iron-containing corundum-high iron mullite solid solution raw material according to claim 4, characterized in that: The regulator is sodium carbonate, the inhibitor is sulfonic acid-phosphoric acid double-modified cellulose, and the collector is a mixture of dodecylamine and sodium oleate, wherein the weight ratio of dodecylamine to sodium oleate is 3:

1.

6. The method for preparing an iron-containing corundum-high iron mullite solid solution raw material according to claim 5, characterized in that: The preparation method of the sulfonic acid-phosphoric acid double-modified cellulose is: The carboxymethyl cellulose is dispersed in deionized water, stirred for 20-40 minutes, and aminosulfonic acid is added. The pH value is adjusted to 5-6 with a 5% sodium hydroxide solution by mass, and the mixture is reacted in a water bath at 60-100° C. for 2-5 hours. The mixture is cooled to room temperature, precipitated and washed with ethanol, and vacuum dried at 50-70° C. to obtain sulfonated carboxymethyl cellulose. The sulfonated carboxymethyl cellulose is mixed with deionized water, sodium tripolyphosphate and urea are added, and the pH value is adjusted to 9-10 with a 5% sodium hydroxide solution by mass, and the mixture is reacted at 70-90° C. for 3-5 hours. The reaction solution is adjusted to a pH value of 7-7.5 with hydrochloric acid, precipitated and washed with ethanol, and dried to obtain sulfonic acid-phosphoric acid double-modified cellulose.

7. The method for preparing an iron-containing corundum-high iron mullite solid solution raw material according to claim 6, characterized in that: The usage ratio of the carboxymethyl cellulose, deionized water and aminosulfonic acid is 8-15g:120-180mL:2-5g; the usage ratio of the sulfonated carboxymethyl cellulose, deionized water, sodium tripolyphosphate and urea is 8-15g:80-150mL:1-5g:0.5-1.0g.

8. The method for preparing an iron-containing corundum-high iron mullite solid solution raw material according to claim 1, characterized in that: In step S3, the filter press is performed using a plate and frame filter press with a pressure set at 0.8-1.2 MPa, and the moisture content of the obtained filter cake is ≤18%. The drying is performed in a rotary drying kiln with a temperature controlled at 200-250° C. for 1-2 hours, and the outlet moisture is ≤1%.

9. The method for preparing an iron-containing corundum-high iron mullite solid solution raw material according to claim 1, characterized in that: The gradient sintering method in step S4 is: Stage 1: room temperature - 600°C, heating rate 2°C / min; Stage 2: 600°C-1450°C, heating rate 5°C / min; Stage 3: 1450℃-1600℃, heating rate is 2℃ / min.

10. The raw material prepared by the method for preparing an iron-containing corundum-high iron mullite solid solution raw material according to any one of claims 1 to 9, characterized in that: Calculated by weight percentage, the invention comprises the following components: 5-30 wt% of silicon dioxide, 5-12 wt% of iron oxide, 1-3 wt% of titanium dioxide, 1-3 wt% of calcium oxide, 0.1-1 wt% of other impurities, and the balance being aluminum oxide.

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