CN114031413A - Production method of acid dry-vibration furnace lining special for metal silicon smelting - Google Patents
Production method of acid dry-vibration furnace lining special for metal silicon smelting Download PDFInfo
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Abstract
A production method of an acid dry-vibration furnace lining special for metal silicon smelting comprises four steps of preparing a sintering aid, mixing a furnace lining material, molding the furnace lining material and sintering the furnace lining material; the chemical formula of the sintering aid is 3Al2O3·17SiO2(ii) a The furnace lining material comprises, by weight, 14-19 parts of fused quartz, 60-74 parts of natural quartz, 0.5-1.5 parts of chromium oxide fine powder, 0.5-1.3 parts of zirconium oxide fine powder, 5-7 parts of silicon carbide fine powder, 2.5-5.0 parts of boron nitride fine powder, 1-2 parts of boric acid and 2.5-4.2 parts of sintering aids; the service temperature of the obtained furnace lining is more than 1700 ℃, the molten iron corrosion resistance index is 2.4-3.7%, and the pressure resistance is realizedThe strength is 51-59 MPa, the heat conductivity coefficient at 600 ℃ is 23.922-28.639W/mK, and the service life of the furnace lining reaches 332-363 furnaces at 1750 ℃.
Description
Technical Field
The invention relates to a production method of an acid dry-vibration furnace lining special for metal silicon smelting, belonging to the field of refractory materials.
Background
When metal silicon is smelted by using a medium-frequency induction furnace, a dry vibrating furnace lining material prepared by adding part of fused quartz into natural quartz is commonly used in the market at present, the conditions of poor volume stability and spalling of the lining material and the intolerance of the furnace bottom caused by special smelting conditions exist, the service life is short, the cost of refractory materials is high, and the frequent repair of the furnace bottom seriously influences the production continuity and the benefit.
Chinese patent CN113548880A discloses an excellent high-strength thermal shock-resistant acidic dry vibrating material and a construction method thereof, wherein the dry vibrating material comprises quartz sand particles, fused quartz sand particles and fine powder. According to the formula, the thermal shock resistance and the density of the furnace lining are improved in a mode of high-purity microcrystalline quartz sand, high-quality fused quartz sand and special compound additives, the refractoriness, the impact strength and the chemical corrosion resistance of the furnace lining are poor, and the cost is relatively high because the high-purity microcrystalline quartz sand and the high-quality fused quartz sand are selected as raw materials.
Chinese patent CN109053172A discloses a dry vibrating material for an intermediate frequency induction furnace, and a preparation method and a use method thereof. According to the preparation method, the extremely high refractoriness of the nano silicon carbide and the graphene can effectively isolate and inhibit carbon in furnace burden (molten iron) from SiO in a furnace lining2The furnace lining obtained in the patent has poor mechanical impact resistance and thermal shock resistance, and the high-cost additive is difficult to bear for the furnace lining material used as a consumable product due to the addition of the graphene with the mass fraction of 5-10 wt%.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a production method of an acid dry-vibration furnace lining special for metal silicon smelting, which realizes the following purposes: the prepared acid dry vibrating furnace lining has high refractoriness, good mechanical impact resistance, good chemical erosion resistance, excellent thermal shock resistance, low cost and high performance, and the use temperature is more than 1700 ℃.
In order to realize the purpose, the invention adopts the following technical scheme:
a process for preparing the acidic dry-vibration furnace liner used for smelting metallic silicon includes preparing sintering assistant, mixing furnace liner, shaping, and calciningKnot four steps; the chemical formula of the sintering aid is 3Al2O3·17SiO2(ii) a The furnace lining material comprises, by weight, 14-19 parts of fused quartz, 60-74 parts of natural quartz, 0.5-1.5 parts of chromium oxide fine powder, 0.5-1.3 parts of zirconium oxide fine powder, 5-7 parts of silicon carbide fine powder, 2.5-5.0 parts of boron nitride fine powder, 1-2 parts of boric acid and 2.5-4.2 parts of sintering aids.
The following is a further improvement of the above technical solution:
step 1 preparation of sintering aid
(1) Preparation of silica-alumina gel
Adding aqueous fumed silica into the potassium silicate aqueous solution, stirring until the solution is transparent, then adding the silicon phosphate aqueous solution, uniformly stirring, increasing to a first stirring speed, slowly adding sodium aluminosilicate powder into the solution, stirring until the solution is in a milky suspension state after the sodium aluminosilicate powder is added, reducing to a second stirring speed, controlling the temperature to be 40-60 ℃, and reacting until the solution is in a gel state to obtain silicon-aluminum gel;
the first stirring speed is 2000-3000 r/min;
the second stirring speed is 400-650 rpm;
the potassium silicate water solution comprises 16-25 wt% of potassium silicate and 2.2-3 of potassium silicate modulus;
the particle size of the aqueous fumed silica is 20nm, and the adding amount of the aqueous fumed silica is 0.8-1.2 wt% of the potassium silicate solution;
the silicon phosphate aqueous solution has a silicon phosphate weight fraction of 13-20 wt% and an addition amount of 12-24 wt% of the potassium silicate aqueous solution;
the particle size of the sodium aluminosilicate powder is 120nm, and the addition amount of the sodium aluminosilicate powder is 6-10 wt% of the potassium silicate aqueous solution.
(2) Drying and sintering
Drying the silicon-aluminum gel at 80-90 ℃ for 3-6 hours, crushing the silicon-aluminum gel into 300-500 mesh powder, heating the powder in a vacuum environment at 400-550 ℃ for 1.5-2.5 hours, crushing the obtained solid into 400-600 mesh powder, namely the sintering aid, wherein the chemical formula is 3Al2O3·17SiO2。
Step 2 furnace lining material mixing
The furnace lining material comprises the following raw material components in parts by weight:
14-19 parts of fused quartz, 60-74 parts of natural quartz, 0.5-1.5 parts of chromium oxide fine powder, 0.5-1.3 parts of zirconium oxide fine powder, 5-7 parts of silicon carbide fine powder, 2.5-5.0 parts of boron nitride fine powder, 1-2 parts of boric acid and 2.5-4.2 parts of sintering aid;
the fused quartz and the natural quartz have the silicon dioxide content of more than 99.5wt%, the alkali metal oxide content of less than 0.15wt% and the ferric oxide content of less than 0.1 wt%;
the fused quartz comprises, by weight, 10-13 parts of fused quartz with the particle size of 1-5 mm and 4-6 parts of fused quartz with the particle size of 150-1000 microns;
the natural quartz comprises, by weight, 16-22 parts of natural quartz with the particle size of 1-5 mm, 21-24 parts of natural quartz with the particle size of 150-1000 microns and 23-28 parts of natural quartz with the particle size of 25-150 microns;
the particle sizes of the chromium oxide fine powder, the zirconium oxide fine powder, the silicon carbide fine powder and the boron nitride fine powder are all 25-150 micrometers;
mixing furnace lining materials: pretreating the furnace lining raw material until the water content is less than 0.3%, adding fused quartz with the particle size of 1-5 mm, natural quartz with the particle size of 1-5 mm, fused quartz with the particle size of 150-1000 microns and natural quartz with the particle size of 150-1000 microns into a forced mixer, fully mixing uniformly, adding natural quartz with the particle size of 25-150 microns, chromium oxide fine powder, zirconium oxide fine powder, silicon carbide fine powder, boron nitride fine powder, sintering aid and boric acid, and continuously stirring and uniformly mixing to obtain the furnace lining.
Step 3 furnace lining forming
Furnace lining molding: building a furnace bottom, filling the prepared furnace lining material on the furnace bottom paved with the glass fiber cloth, filling for three times, exhausting for 4-6 times by using an exhaust fork after adding the material each time, vibrating for 20-30 minutes by using a furnace bottom vibrator to scrape out a material with the thickness of 2cm on the surface, putting into a steel die, building a furnace wall, fully scraping the bonding position of the furnace bottom material and the furnace wall material, then adding the furnace lining material layer by layer, exhausting for 5-7 times by using the exhaust fork for each layer, vibrating the steel die by using the furnace wall vibrator for each layer for 15-25 minutes, and compacting for each layer to have the thickness of 15 cm.
Step 4 sintering of furnace lining
Sintering a furnace lining: after the furnace building is finished, heating to 950-1050 ℃ at the speed of 30-40 ℃/h, keeping the temperature for 2-3 hours, rapidly cooling, taking out a steel die, adding a smelting raw material, heating to slowly melt the raw material to a liquid state, heating to 1600-1750 ℃ after the furnace is full, and keeping the temperature for 2-4 hours to fully sinter the furnace lining material.
Compared with the prior art, the invention has the following beneficial effects:
1. the acid dry-vibration furnace lining obtained by the production method has high refractoriness, the service temperature is over 1700 ℃, and the service life of the furnace lining reaches 332-363 furnaces at the service temperature of 1750 ℃;
2. the acidic dry-vibration furnace lining obtained by the production method has good mechanical impact resistance and compressive strength of 51-59 MPa;
3. the acidic dry-vibration furnace lining obtained by the production method has good chemical erosion resistance, and the molten iron corrosion resistance index is 2.4-3.7%;
4. the acid dry-vibration furnace lining obtained by the production method has excellent thermal shock resistance, and the thermal conductivity coefficient at 600 ℃ is 23.922-28.639W/mK;
5. according to the production method, the mass of the natural quartz in the furnace lining material formula is 60-74 wt%, the cost of the raw materials is low, and the cost of the final acid dry-vibration furnace lining product can be greatly reduced.
Detailed Description
The following description of the preferred embodiments of the present invention is provided for the purpose of illustration and description, and is in no way intended to limit the invention.
Example 1: production method of acid dry-vibration furnace lining special for metal silicon smelting
The method comprises the following steps:
1. preparation of sintering aid
(1) Preparation of silica-alumina gel
Adding 1.2 kg of aqueous fumed silica into 120 kg of 21% potassium silicate aqueous solution by mass concentration, stirring until the solution is transparent, then adding 24 kg of 18% silicon phosphate aqueous solution by mass fraction, uniformly stirring, controlling the stirring speed to 2600 r/min, slowly adding 8.4 kg of sodium aluminosilicate powder into the solution, stirring until the solution is in a milky suspension state after the addition is finished, controlling the stirring speed to 500 r/min and the temperature to 52 ℃, and reacting until the solution is in a gel state to obtain the silica-alumina gel;
the modulus of the potassium silicate aqueous solution is 2.8;
the particle size of the aqueous fumed silica is 20 nm;
the particle size of the sodium aluminosilicate powder is 120 nm;
(2) drying and sintering
Drying the silicon-aluminum gel at 87 ℃ for 5 hours, crushing the silicon-aluminum gel into 400-mesh powder, heating the powder in a 480 ℃ vacuum environment for 2 hours, and crushing the obtained solid into 500-mesh powder, namely the sintering aid.
2. Furnace lining material mixing
Drying fused quartz, natural quartz, chromium oxide fine powder, zirconium oxide fine powder, silicon carbide fine powder, boron nitride fine powder, boric acid and sintering aid until the water content is less than 0.3%, adding 12 parts of fused quartz with the particle size of 1-5 mm, 19 parts of natural quartz with the particle size of 1-5 mm, 5 parts of fused quartz with the particle size of 150-1000 microns and 22 parts of natural quartz with the particle size of 150-1000 microns into a forced mixer, fully mixing uniformly, adding 25 parts of natural quartz with the particle size of 25-150 microns, 1.2 parts of chromium oxide fine powder, 1 part of zirconium oxide fine powder, 6 parts of silicon carbide fine powder, 3.8 parts of boron nitride fine powder, 3.5 parts of sintering aid and 1.5 parts of boric acid, and continuously stirring and uniformly mixing to obtain a furnace lining material;
the particle sizes of the chromium oxide fine powder, the zirconium oxide fine powder, the silicon carbide fine powder and the boron nitride fine powder are all 25-150 micrometers.
3. Furnace lining forming and sintering
Furnace lining molding: building a furnace bottom, filling prepared furnace lining materials on the furnace bottom paved with the glass fiber cloth, filling for three times, vibrating for 26 minutes by using a furnace bottom vibrator after exhausting for 5 times by using an exhaust fork after adding materials each time, scraping materials with the thickness of 2cm on the surface, placing the materials into a steel mould, starting building a furnace wall, fully scraping the combination position of furnace bottom materials and furnace wall materials, then adding the furnace lining materials layer by layer, exhausting for 6 times by using the exhaust fork for each layer, vibrating the steel mould by using the furnace wall vibrator, vibrating for 20 minutes for each layer, and compacting for 15cm in each layer thickness;
4. sintering a furnace lining: after the furnace building is finished, heating to 1020 ℃ at the temperature of 33 ℃/hour, keeping the temperature constant for 2.8 hours, rapidly cooling, taking out a steel die, adding a smelting raw material, slowly melting to a liquid state, increasing the temperature to 1700 ℃ after the furnace is filled, and preserving the heat for 3.5 hours to fully sinter the furnace lining material.
Example 2: production method of acid dry-vibration furnace lining special for metal silicon smelting
The method comprises the following steps:
1. preparation of sintering aid
(1) Preparation of silica-alumina gel
Adding 0.96 kg of aqueous fumed silica into 120 kg of 16% potassium silicate aqueous solution by mass concentration, stirring until the solution is transparent, then adding 14.4 kg of 13% silicon phosphate aqueous solution by mass fraction, uniformly stirring, controlling the stirring speed to be 2000 rpm, slowly adding 7.2 kg of sodium aluminosilicate powder into the solution, stirring until the solution is in a milky suspension state after the addition is finished, controlling the stirring speed to be 400 rpm and the temperature to be 40 ℃, and reacting until the solution is in a gel state to obtain the silica-alumina gel;
the modulus of the potassium silicate aqueous solution is 2.2;
the particle size of the aqueous fumed silica is 20 nm;
the particle size of the sodium aluminosilicate powder is 120 nm;
(2) drying and sintering
Drying the silicon-aluminum gel at 80 ℃ for 3 hours, crushing the silicon-aluminum gel into 300-mesh powder, heating the powder at 400 ℃ for 1.5 hours in a vacuum environment, and crushing the obtained solid into 400-mesh powder again, namely the sintering aid.
2. Furnace lining material mixing
Drying fused quartz, natural quartz, chromium oxide fine powder, zirconium oxide fine powder, silicon carbide fine powder, boron nitride fine powder, boric acid and sintering aid until the water content is less than 0.3%, adding 13 parts of fused quartz with the particle size of 1-5 mm, 22 parts of natural quartz with the particle size of 1-5 mm, 6 parts of fused quartz with the particle size of 150-1000 microns and 24 parts of natural quartz with the particle size of 150-1000 microns into a forced mixer, fully mixing uniformly, adding 23 parts of natural quartz with the particle size of 25-150 microns, 0.5 part of chromium oxide fine powder, 0.5 part of zirconium oxide fine powder, 5 parts of silicon carbide fine powder, 2.5 parts of boron nitride fine powder, 2.5 parts of sintering aid and 1 part of boric acid, and continuously stirring and uniformly mixing to obtain a furnace lining material;
the particle sizes of the chromium oxide fine powder, the zirconium oxide fine powder, the silicon carbide fine powder and the boron nitride fine powder are all 25-150 micrometers.
3. Furnace lining molding: building a furnace bottom, filling the prepared furnace lining material on the furnace bottom paved with the glass fiber cloth, filling the furnace lining material for three times, vibrating the furnace lining material for 20 minutes by using a furnace bottom vibrator after exhausting the material for 4 times by using an exhaust fork each time, scraping the material with the thickness of 2cm on the surface, putting the furnace bottom into a steel die, building a furnace wall, fully scraping the binding position of the furnace bottom material and the furnace wall material, then adding the furnace lining material layer by layer, exhausting the material for 5 times by using the exhaust fork for each layer, vibrating the steel die by using the furnace wall vibrator, vibrating the steel die for each layer for 15 minutes, and compacting the thickness of each layer for 15 cm.
4. Sintering a furnace lining: after the furnace building is finished, heating to 950 ℃ at the temperature of 30 ℃/hour, keeping the temperature for 2 hours, rapidly cooling, taking out a steel die, adding a smelting raw material, slowly melting to a liquid state, increasing the temperature to 1600 ℃ after the furnace is filled, and preserving the heat for 2 hours to fully sinter the furnace lining material.
Example 3: production method of acid dry-vibration furnace lining special for metal silicon smelting
The method comprises the following steps:
1. preparation of sintering aid
(1) Preparation of silica-alumina gel
Adding 1.44 kg of aqueous fumed silica into 120 kg of 25% potassium silicate aqueous solution by mass concentration, stirring until the solution is transparent, then adding 15.6 kg of 20% silicon phosphate aqueous solution by mass fraction, uniformly stirring, controlling the stirring speed to 3000 r/min, slowly adding 12 kg of sodium aluminosilicate powder into the solution, stirring until the solution is in a milky suspension state after the addition is finished, controlling the stirring speed to 650 r/min and the temperature to 60 ℃, and reacting until the solution is in a gel state to obtain the silica-alumina gel;
the modulus of the potassium silicate aqueous solution is 2.2;
the particle size of the aqueous fumed silica is 20 nm;
the particle size of the sodium aluminosilicate powder is 120 nm;
(2) drying and sintering
Drying the silicon-aluminum gel at 90 ℃ for 6 hours, crushing the silicon-aluminum gel into 500-mesh powder, heating the powder at 550 ℃ for 2.5 hours in a vacuum environment, and crushing the obtained solid into 600-mesh powder, namely the sintering aid.
2. Furnace lining material mixing
Drying fused quartz, natural quartz, chromium oxide fine powder, zirconium oxide fine powder, silicon carbide fine powder, boron nitride fine powder, boric acid and sintering aid until the water content is less than 0.3%, adding 10 parts of fused quartz with the particle size of 1-5 mm, 16 parts of natural quartz with the particle size of 1-5 mm, 4 parts of fused quartz with the particle size of 150-1000 microns and 21 parts of natural quartz with the particle size of 150-1000 microns into a forced mixer, fully mixing uniformly, adding 28 parts of natural quartz with the particle size of 25-150 microns, 1.5 parts of chromium oxide fine powder, 1.3 parts of zirconium oxide fine powder, 7 parts of silicon carbide fine powder, 5 parts of boron nitride fine powder, 4.2 parts of sintering aid and 2 parts of boric acid, and continuously stirring and uniformly mixing to obtain a furnace lining material;
the particle sizes of the chromium oxide fine powder, the zirconium oxide fine powder, the silicon carbide fine powder and the boron nitride fine powder are all 25-150 micrometers.
3. Furnace lining molding: building a furnace bottom, filling the prepared furnace lining material on the furnace bottom paved with the glass fiber cloth, filling for three times, vibrating for 30 minutes by using a furnace bottom vibrator after exhausting for 4 times by using an exhaust fork after adding the material each time, scraping out a material with the thickness of 2cm on the surface, placing the material into a steel mould, starting building a furnace wall, fully scraping the binding position of the furnace bottom material and the furnace wall material, then adding the furnace lining material layer by layer, exhausting for 7 times by using the exhaust fork for each layer, vibrating the steel mould by using the furnace wall vibrator, vibrating for 25 minutes for each layer, and compacting for each layer to have the thickness of 15 cm;
4. sintering a furnace lining: after the furnace building is finished, heating to 1050 ℃ at the temperature of 40 ℃/hour, keeping the temperature constant for 3 hours, rapidly cooling, taking out a steel die, adding a smelting raw material, slowly melting to a liquid state, increasing the temperature to 1750 ℃ after the furnace is filled, and preserving the heat for 4 hours to fully sinter the furnace lining material.
And (3) furnace lining performance test:
1. chemical resistance: testing the molten iron corrosion resistance index of the furnace lining according to the GB/T24201-2009 standard;
2. mechanical impact resistance: testing the compressive strength of the furnace lining according to GB/T5072-2008 standard;
3. thermal shock resistance: testing the heat conductivity coefficient of the furnace lining according to GB/T37796 and 2019 standards;
the test data are shown in the following table:
Claims (10)
1. a production method of an acid dry-vibration furnace lining special for metal silicon smelting is characterized by comprising the following steps: the method comprises four steps of preparing a sintering aid, mixing furnace lining materials, forming a furnace lining and sintering the furnace lining;
the chemical formula of the sintering aid is 3Al2O3·17SiO2；
The furnace lining material comprises, by weight, 14-19 parts of fused quartz, 60-74 parts of natural quartz, 0.5-1.5 parts of chromium oxide fine powder, 0.5-1.3 parts of zirconium oxide fine powder, 5-7 parts of silicon carbide fine powder, 2.5-5.0 parts of boron nitride fine powder, 1-2 parts of boric acid and 2.5-4.2 parts of sintering aids.
2. The production method of the special acid dry vibration furnace lining for the metal silicon smelting according to claim 1, which is characterized in that: the preparation of the sintering aid comprises the steps of preparing silicon-aluminum gel and drying and sintering; the preparation method comprises the steps of adding aqueous fumed silica into a potassium silicate aqueous solution, stirring until the solution is transparent, then adding a silicon phosphate aqueous solution, uniformly stirring, increasing the stirring speed to a first stirring speed, slowly adding sodium aluminosilicate powder into the solution, stirring until the solution is in a milky suspension state, reducing the stirring speed to a second stirring speed, controlling the temperature to be 40-60 ℃, and reacting until the solution is in a gel state to obtain the silicon-aluminum gel.
3. The production method of the special acid dry vibration furnace lining for the metal silicon smelting according to claim 2, which is characterized in that: the first stirring speed is 2000-3000 r/min; the second stirring speed is 400-650 rpm.
4. The production method of the special acid dry vibration furnace lining for the metal silicon smelting according to claim 2, which is characterized in that: the potassium silicate water solution comprises 16-25 wt% of potassium silicate and 2.2-3 of potassium silicate modulus;
the particle size of the aqueous fumed silica is 20nm, and the addition amount of the aqueous fumed silica is 0.8-1.2 wt% of the potassium silicate solution.
5. The production method of the special acid dry vibration furnace lining for the metal silicon smelting according to claim 2, which is characterized in that: the silicon phosphate aqueous solution has a silicon phosphate weight fraction of 13-20 wt% and an addition amount of 12-24 wt% of the potassium silicate aqueous solution;
the particle size of the sodium aluminosilicate powder is 120nm, and the addition amount of the sodium aluminosilicate powder is 6-10 wt% of the potassium silicate aqueous solution.
6. The production method of the special acid dry vibration furnace lining for the metal silicon smelting according to claim 2, which is characterized in that: and drying and sintering, namely drying the silicon-aluminum gel at 80-90 ℃ for 3-6 hours, crushing the silicon-aluminum gel into 300-500-mesh powder, heating the powder in a vacuum environment at 400-550 ℃ for 1.5-2.5 hours, and crushing the obtained solid into 400-600-mesh powder, namely the sintering aid.
7. The production method of the special acid dry vibration furnace lining for the metal silicon smelting according to claim 1, which is characterized in that: the fused quartz and the natural quartz have the silicon dioxide content of more than 99.5wt%, the alkali metal oxide content of less than 0.15wt% and the ferric oxide content of less than 0.1 wt%.
8. The production method of the special acid dry vibration furnace lining for the metal silicon smelting according to claim 1, which is characterized in that: the fused quartz comprises, by weight, 10-13 parts of fused quartz with the particle size of 1-5 mm and 4-6 parts of fused quartz with the particle size of 150-1000 microns;
the natural quartz comprises, by weight, 16-22 parts of natural quartz with the particle size of 1-5 mm, 21-24 parts of natural quartz with the particle size of 150-1000 microns and 23-28 parts of natural quartz with the particle size of 25-150 microns.
9. The production method of the special acid dry vibration furnace lining for the metal silicon smelting according to claim 1, which is characterized in that: the particle sizes of the chromium oxide fine powder, the zirconium oxide fine powder, the silicon carbide fine powder and the boron nitride fine powder are all 25-150 micrometers.
10. The production method of the special acid dry vibration furnace lining for the metal silicon smelting according to claim 1, which is characterized in that: the furnace lining material is mixed, the furnace lining material is pretreated until the water content is less than 0.3%, fused quartz with the particle size of 1-5 mm, natural quartz with the particle size of 1-5 mm, fused quartz with the particle size of 150-1000 microns and natural quartz with the particle size of 150-1000 microns are added into a forced mixer to be fully mixed, natural quartz with the particle size of 25-150 microns, chromium oxide fine powder, zirconium oxide fine powder, silicon carbide fine powder, boron nitride fine powder, sintering aid and boric acid are added, and the furnace lining material is obtained after continuous stirring and mixing.
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