CN115385673A - High-strength silica brick for hydrogen metallurgy and preparation method thereof - Google Patents
High-strength silica brick for hydrogen metallurgy and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a high-strength silica brick for hydrogen metallurgy and a preparation method thereof. A preparation method of a high-strength silica brick for hydrogen metallurgy uses 85-95 wt% of silica, 1-3 wt% of silicon micropowder, 1-3 wt% of lime milk, 0.5-7 wt% of silicon carbide and 0.5-7 wt% of zirconium oxide as raw materials, and comprises the steps of mixing, adding 1-5 wt% of sulfurous acid pulp waste liquor, mixing, press forming, drying and calcining to obtain the high-strength silica brick for hydrogen metallurgy. The high-strength silicon brick for hydrogen metallurgy prepared by the invention has good thermal shock stability and H resistance 2 ‑H 2 O gas has strong corrosion performance and is suitable for adopting H 2 Or H 2 And + the hydrogen metallurgy natural gas-based shaft furnace iron making with CO mixed gas as a reducing agent.
Description
Technical Field
The invention relates to the technical field of silica bricks, in particular to a high-strength silica brick for hydrogen metallurgy and a preparation method thereof.
Background
The hydrogen metallurgy is a technology for obtaining a solid iron-containing material in a temperature range lower than the melting point of iron by using hydrogen to partially or completely replace carbon as a reducing agent of iron ore. High purity H 2 At 8The temperature is kept at 00 ℃ for 6 hours, and the iron ore can be completely reduced into Fe. The silica brick has the characteristics of small high-temperature volume expansibility and acid slag resistance, and is expected to be used for the shaft furnace for hydrogen metallurgy.
The silica brick has the characteristics of high refractoriness under load, small volume expansion at high temperature and acid slag resistance, and is used for the natural gas-based shaft furnace for hydrogen metallurgy. The main raw material of the silica brick is silica which is easy to generate crystal transformation and volume expansion in the high-temperature sintering process; at the same time, siO 2 Among various crystal forms, tridymite has a 'spearhead twin' structure, and is beneficial to improving mechanical properties. In order to promote the generation of tridymite in the preparation process of the silica brick, a mineralizer is generally required to be added, and the mineralizer can be mixed with SiO 2 The reaction produces a liquid phase, which accelerates the formation of tridymite and reduces thermal stress. Sunyao et al (Sunyao, dian sprout, zhao Peng Fei, etc. Shandong Metallurgical, 2018,40 (3): 27-29.) adopt lime milk as mineralizer to promote the generation of tridymite during the firing process of silica brick; manivasakan et al (Manivasakan P, rajendran V, rauta P R, et al. Journal of the American Ceramic Society,2010,93 (8): 2236-2243.) prepared silica bricks having a refractoriness under load of 1680 ℃ by incubating at 1450 ℃ for 32 hours using lime and iron oxide as mineralizers. From the above technology, it can be seen that the mineralizer used in the current silica brick production process further promotes the generation of tridymite to improve the mechanical properties. However, the silica brick has good thermal shock stability at high temperature, and SiO in the silica brick is in service at medium and low temperature 2 The crystal transformation occurs to generate volume change, so that the thermal shock stability is poor, and the silicon brick can generate cracks and be peeled off after being cooled once at 1000 ℃ by water. H 2 The iron ore is reduced, the reaction can be started at 570 ℃, high-purity Fe can be obtained by keeping the temperature at 800 ℃ for 8 hours, and the application of the silica brick in the field of hydrogen metallurgy is limited by the characteristic of poor thermal shock stability under the condition of medium and low temperature.
Disclosure of Invention
The invention aims to provide a high-strength silica brick for hydrogen metallurgy and a preparation method thereof aiming at the defects of the prior art, and the high-strength silica brick for hydrogen metallurgy prepared by the method has good thermal shock stability and H resistance 2 -H 2 And the corrosion performance of O gas is strong.
The invention relates to a preparation method of a high-strength silica brick for hydrogen metallurgy, which takes 85-95 wt% of silica, 1-3 wt% of silicon micropowder, 1-3 wt% of lime milk, 0.5-7 wt% of silicon carbide and 0.5-7 wt% of zirconia as raw materials, mixes the raw materials, adds 1-5 wt% of sulfurous acid pulp waste liquor of the raw materials, mixes, presses and forms, and calcines the raw materials after drying to prepare the high-strength silica brick for hydrogen metallurgy; then, the high-strength silica brick for hydrogen metallurgy is prepared.
Furthermore, the calcination is carried out in a high temperature furnace, the temperature is raised to 1380-1500 ℃ at the speed of 5-12 ℃/h, and the temperature is kept for 8-14 h.
Further, siO of the silica particles 2 The content is more than or equal to 98wt%; the silica has a particle size distribution of:
the silica having a particle size of less than 5mm and not less than 3mm accounts for 20 to 30wt%,
40 to 55wt% of silica having a particle diameter of less than 3mm and not less than 1mm,
the particle size of less than 0.088mm accounts for 20-32 wt% of silica.
Further, siO of the silicon micropowder 2 The content is more than or equal to 92wt%, and the grain diameter of the silicon micro powder is less than or equal to 0.6 mu m.
Further, caO of the lime milk is more than or equal to 60wt%.
Further, the SiC content of the silicon carbide is more than or equal to 98wt%, and the grain diameter of the silicon carbide is less than or equal to 74 mu m.
Further, zrO of the zirconia 2 The content is more than or equal to 99wt%, and the particle size of the zircon is less than or equal to 74 mu m.
The high-strength silicon brick for hydrogen metallurgy prepared by the preparation method.
Due to the adoption of the technical scheme, compared with the prior art, the invention has the following positive effects:
silicon carbide and zirconia are added into the silica brick, siC can be oxidized in the high-temperature sintering process, and under the condition of higher oxygen partial pressure, dense SiO is firstly generated on the SiC surface 2 Protective layer of SiO 2 A SiC-wrapped structure; as the oxidation process continues, oxygen in the air needs to diffuse through the SiO 2 The protective layer continuously oxidizes the internal SiC,SiO 2 Presence of a protective layer, resulting in diffusion of O into the inner layer in contact with SiC 2 The inner SiC layer is passively oxidized to generate SiO (g) gas under the condition of low partial pressure and low partial pressure, the inner SiC layer disappears to form pores, and SiO on the outer part 2 The protective layer reacts with the zirconium oxide to generate ZrSiO 4 Wrapping the inner pores to finally form the micro-pores ZrSiO 4 A binding phase; zrSiO of micropore structure 4 The binding phase has more micro air holes which can absorb SiO in the service process of the silica brick 2 The phase change generates volume expansion and thermal stress, and the thermal shock stability is greatly improved. And ZrSiO 4 The binding phase itself has excellent H resistance 2 -H 2 ZrSiO of O-corrosive, microporous structure 4 The binding phase can complicate the pore structure of silica brick, prolong the gas diffusion path, prevent corrosive gas from permeating into the material, and improve the H resistance 2 -H 2 O-coupled gas corrosiveness.
The high-strength silica brick for hydrogen metallurgy prepared by the invention is detected as follows: thermal shock (firstly heating to 1100 ℃ and preserving heat for 30min, then putting into flowing water for cooling) cycle times of 16-26 times, and the refractoriness under load under 0.2MPa is 1679-1700 ℃; the normal temperature compressive strength is 62-95 MPa; passing through H at 900 DEG C 2 -H 2 After the O mixed gas is corroded for 10 hours, the compressive strength is 48-80 MPa.
Therefore, the high-strength silica brick for hydrogen metallurgy prepared by the invention has good thermal shock stability and H resistance 2 -H 2 O gas has strong corrosion performance and is suitable for adopting H 2 Or H 2 And (4) making iron by using the hydrogen metallurgy natural gas-based shaft furnace with the CO mixed gas as a reducing agent.
Detailed Description
The following are specific examples of the present invention and further describe the technical solutions of the present invention, but the present invention is not limited to these examples.
The invention is further described with reference to specific embodiments, without limiting its scope.
In order to avoid repetition, the materials used in this embodiment are described in a unified manner as follows, which is not described in the embodiment again:
SiO of the silica 2 The content is more than or equal to 98wt%; the silica has a particle size distribution of:
the silica having a particle size of less than 5mm and not less than 3mm accounts for 20 to 30wt%,
the silica having a particle diameter of less than 3mm and not less than 1mm accounts for 40 to 55wt%,
the particle size of less than 0.088mm accounts for 20-32 wt% of silica.
SiO of the silicon micropowder 2 The content is more than or equal to 92wt%; the grain diameter of the silicon micro powder is less than or equal to 0.6 mu m.
The CaO of the lime milk is more than or equal to 60wt%.
The SiC content of the silicon carbide is more than or equal to 98wt%; the grain diameter of the silicon carbide is less than or equal to 74 mu m.
ZrO of the zirconia 2 The content is more than or equal to 99wt%; the grain diameter of the zirconia is less than or equal to 74 mu m.
Example 1
A high-strength silica brick for hydrogen metallurgy and a preparation method thereof. The preparation method in this example is:
taking 85-90 wt% of silica, 1-2 wt% of silicon powder, 1-3 wt% of lime milk, 3-7 wt% of silicon carbide and 3-7 wt% of zirconium oxide as raw materials, mixing, adding 1-5 wt% of sulfurous acid paper pulp waste liquor of the raw materials, mixing, press forming and drying; then placing the mixture into a high-temperature furnace, raising the temperature to 1430-1500 ℃ at the speed of 5-10 ℃/h, and preserving the temperature for 10-14 h to obtain the high-strength silica brick for hydrogen metallurgy.
The high-strength silica brick for hydrogen metallurgy prepared by the embodiment is detected: thermal shock (firstly heating to 1100 ℃ and preserving heat for 30min, then putting into flowing water for cooling) cycle times of 22-26 times, and the refractoriness under load under 0.2MPa is 1696-1700 ℃; the normal temperature compressive strength is 87-95 MPa; passing through H at 900 deg.C 2 -H 2 After the O mixed gas is corroded for 10 hours, the compressive strength is 69-80 MPa.
Example 2
A high-strength silica brick for hydrogen metallurgy and a preparation method thereof. The preparation method in this example is:
mixing 88-91 wt% of silica, 1-2 wt% of silicon powder, 2-3 wt% of lime milk, 2-6 wt% of silicon carbide and 2-6 wt% of zirconium oxide, adding 1-5 wt% of sulfurous acid pulp waste liquor, mixing, press-forming and drying; then placing the mixture into a high-temperature furnace, raising the temperature to 1430-1500 ℃ at the speed of 5-10 ℃/h, and preserving the temperature for 10-14 h to obtain the high-strength silica brick for hydrogen metallurgy.
The high-strength silica brick for hydrogen metallurgy prepared by the embodiment is detected: the cycle times of thermal shock (firstly heating to 1100 ℃ and preserving the temperature for 30min, then putting into flowing water for cooling) are 19-23 times, and the refractoriness under load under 0.2MPa is 1690-1696 ℃; the normal temperature compressive strength is 80-88 MPa; passing through H at 900 DEG C 2 -H 2 After the O mixed gas is corroded for 10 hours, the compressive strength is 62-71 MPa.
Example 3
A high-strength silica brick for hydrogen metallurgy and a preparation method thereof. The preparation method in this example is:
taking 90-93 wt% of silica, 2-3 wt% of silicon powder, 2.5-4 wt% of lime milk, 1-4 wt% of silicon carbide and 1-4 wt% of zirconia as raw materials, mixing, adding 1-5 wt% of sulfurous acid pulp waste liquor of the raw materials, mixing, pressing for forming and drying; then placing the mixture into a high-temperature furnace, raising the temperature to 1380-1450 ℃ at the speed of 9-12 ℃/h, and preserving the temperature for 8-12 h to prepare the high-strength silicon brick for hydrogen metallurgy.
The high-strength silica brick for hydrogen metallurgy prepared by the embodiment is detected as follows: thermal shock (firstly heating to 1100 ℃ and preserving heat for 30min, then putting into flowing water for cooling) cycle times of 17-20 times, and the refractoriness under load under 0.2MPa is 1685-1693 ℃; the normal temperature compressive strength is 71-82 MPa; passing through H at 900 deg.C 2 -H 2 After the O mixed gas is corroded for 10 hours, the compressive strength is 52-64 MPa.
Example 4
A high-strength silica brick for hydrogen metallurgy and a preparation method thereof. The preparation method in this example is:
using 93-95 wt% of silica, 2-3 wt% of silicon powder, 1-2 wt% of lime milk, 0.5-3 wt% of silicon carbide and 0.5-3 wt% of zirconium oxide as raw materials, mixing, adding 1-5 wt% of sulfurous acid paper pulp waste liquor, mixing, press-forming and drying; then placing the mixture into a high-temperature furnace, raising the temperature to 1380-1450 ℃ at the speed of 9-12 ℃/h, and preserving the temperature for 8-12 h to prepare the high-strength silicon brick for hydrogen metallurgy.
The high-strength silica brick for hydrogen metallurgy prepared by the embodiment is detected as follows: thermal shock (firstly heating to 1100 ℃ and preserving heat for 30min, then putting into flowing water for cooling) cycle times of 16-18 times, wherein the refractoriness under 0.2MPa is 1679-1688 ℃; the normal temperature compressive strength is 62-72 MPa; passing through H at 900 deg.C 2 -H 2 After the O mixed gas is corroded for 10 hours, the compressive strength is 48-55 MPa.
The above is not relevant and is applicable to the prior art.
While certain specific embodiments of the present invention have been described in detail by way of illustration, it will be understood by those skilled in the art that the foregoing is illustrative only and is not limiting of the scope of the invention, as various modifications or additions may be made to the specific embodiments described and substituted in a similar manner by those skilled in the art without departing from the scope of the invention as defined in the appending claims. It should be understood by those skilled in the art that any modifications, equivalents, improvements and the like made to the above embodiments in accordance with the technical spirit of the present invention are included in the scope of the present invention.
Claims (8)
1. A preparation method of a high-strength silica brick for hydrogen metallurgy is characterized by comprising the following steps: taking 85-95 wt% of silica, 1-3 wt% of silicon powder, 1-3 wt% of lime milk, 0.5-7 wt% of silicon carbide and 0.5-7 wt% of zirconia as raw materials, mixing, adding 1-5 wt% of sulfurous acid paper pulp waste liquor of the raw materials, mixing, pressing and molding, drying and calcining to prepare the high-strength silicon brick for hydrogen metallurgy; then, the high-strength silica brick for hydrogen metallurgy is prepared.
2. The method for preparing a high-strength silica brick for hydrogen metallurgy according to claim 1, wherein the calcination is carried out in a high-temperature furnace at a temperature rising rate of 5-12 ℃/h to 1380-1500 ℃ and a temperature holding time of 8-14 h.
3. The method for producing a high-strength silica brick for hydrometallurgy according to claim 1, wherein SiO of the silica particles 2 The content is more than or equal to 98wt%; the silica has a particle size distribution of:
20 to 30wt% of silica having a particle diameter of less than 5mm and not less than 3mm,
the silica having a particle diameter of less than 3mm and not less than 1mm accounts for 40 to 55wt%,
the particle size of less than 0.088mm accounts for 20-32 wt% of silica.
4. The method for producing a high-strength silica brick for use in hydrometallurgy according to claim 1, wherein said fine silica powder is SiO 2 The content is more than or equal to 92wt percent, and the grain diameter of the silicon micro powder is less than or equal to 0.6 mu m.
5. The method for preparing the high-strength silica brick for hydrogen metallurgy according to claim 1, wherein CaO of the lime milk is not less than 60wt%.
6. The method for preparing the high-strength silicon brick for hydrogen metallurgy according to claim 1, wherein the SiC content of the silicon carbide is not less than 98wt%, and the particle size of the silicon carbide is not more than 74 μm.
7. The method for producing a high-strength silica brick for hydrometallurgy according to claim 1, wherein ZrO of the zirconia is ZrO 2 The content is more than or equal to 99wt%, and the particle size of the zircon is less than or equal to 74 mu m.
8. A high-strength silica brick for hydrometallurgy, which is produced by the production method according to any one of claims 1 to 7.
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