Method for preparing black microlite from molten ferronickel slag

Abstract

The invention discloses a method for preparing black microlite from molten ferronickel slag, which comprises the following steps: mixing the molten ferronickel slag with a hardening and tempering agent, and carrying out melting and heat preservation to obtain a homogenized molten mass; casting the homogenized molten mass into a mold to obtain a formed sample; carrying out crystallization treatment on the formed sample under the condition of a non-oxidizing atmosphere, and cooling to obtain black microlite; and the utilization rate of the ferronickel slag is effectively improved.

Description

Technical Field

[0001] The present application relates to a method for preparing black microcrystalline glass from molten nickel-iron slag, belonging to the technical field of comprehensive utilization of resources. Background Art

[0002] Industrial waste residues are characterized by large output, various types, difficult flowability, large composition fluctuations, etc., and are difficult to handle. Nickel-iron slag is a solid waste residue generated during the smelting of nickel-iron alloy. As a by-product of the smelting process, a large amount of stacking not only occupies land resources but also poses a risk of heavy metal pollution. In the prior art, converting nickel-iron slag into microcrystalline glass materials is one of the main research directions. The patent with the publication number CN101020968A discloses a process for preparing microcrystalline glass using high-temperature molten nickel-iron slag. Most of the iron and nickel are extracted by reduction under high-temperature conditions, and the sensible heat of the molten slag is utilized to prepare a microcrystalline glass composite material from the remaining silicate molten slag. However, this method has the following defects: an independent iron extraction by reduction process needs to be set up, resulting in a significant increase in equipment complexity and energy consumption; the nucleation ability of the residual molten slag is insufficient, and expensive nucleating agents need to be relied on to induce crystallization, resulting in an increase in production cost.

[0003] There is a huge market demand for black microcrystalline glass, but the existing preparation technologies still have obvious limitations. The patent with the publication number CN106242301A discloses a method for preparing black microcrystalline glass bricks using liquid converter steel slag as the main raw material, which improves the utilization rate of converter steel slag and fully utilizes the sensible heat of the steel slag to prepare black microcrystalline glass bricks with better wear resistance and rolling resistance. However, this process adds precious metal oxides such as cobalt oxide and nickel oxide as colorants, which increases the production cost to a certain extent. Moreover, iron oxide and manganese oxide are mostly present in the composition of the existing black microcrystalline glass. When prepared in an air atmosphere, the surface of the microcrystalline glass is prone to oxidation, resulting in color change, such as the appearance of miscellaneous colors such as red on the surface, and the color is mottled and impure, affecting the application range of the sample. Summary of the Invention

[0004] The purpose of the present application is to overcome the deficiencies in the prior art and provide a method for preparing black microcrystalline glass from molten nickel-iron slag, which reduces the production cost and improves the utilization rate of nickel-iron slag.

[0005] To achieve the above purpose, the present application is implemented by adopting the following technical solutions: Provide a method for preparing black microcrystalline glass from molten nickel-iron slag, including: Mix molten nickel-iron slag and a conditioning agent in a mass composition ratio of 7:3 to 19:1, and perform melting and heat preservation to obtain a homogenized melt; Cast the homogenized melt into a mold to obtain a formed sample; The formed sample is subjected to crystallization treatment under the condition of a non-oxidizing atmosphere, and then cooled to obtain black microcrystalline glass.

[0006] Furthermore, the temperature range of the crystallization treatment is 800°C to 950°C, and the time is 5 minutes to 60 minutes.

[0007] Furthermore, the temperature range of the melting and holding is 1442°C to 1568°C, and the holding time is 30 minutes to 150 minutes; When casting, the viscosity of the homogenized melt is 0.1 Pa·s to 2.2 Pa·s.

[0008] Furthermore, the molten nickel iron slag includes the following chemical components by mass percentage: SiO2: 40% to 60%, MgO: 20% to 40%, Fe2O3: 1% to 10%, FeO: 1% to 5%, Al2O3: 2% to 8%, CaO: 0.1% to 5%, Cr2O3: 0.1% to 5%, MnO: 0.1% to 1%, Na2O and K2O: 0.01% to 0.5%, and the rest are impurities.

[0009] Furthermore, the homogenized melt includes the following chemical components by mass percentage: SiO2: 48% to 60%, MgO: 18% to 38%, Fe2O3: 4% to 13%, FeO: 1% to 5%, Al2O3: 4% to 11%, CaO: 0.5% to 6%, B2O3: 0% to 6%, Cr2O3: 0.1% to 5%, MnO: 0.1% to 1%, Na2O and K2O: 0.01% to 0.5%.

[0010] Furthermore, the conditioning agent includes a composition adjustment raw material and a clarification raw material; among them, the mass of the composition adjustment raw material is 98% to 100% of the mass of the conditioning agent, and the mass of the clarification raw material is 0 to 2% of the mass of the conditioning agent.

[0011] Furthermore, the composition adjustment raw material is any one or more of limestone, quartz sand, borax, and bauxite powder; the clarification raw material is a mixture of one or more of industrial-grade antimony oxide and industrial-grade sodium chloride.

[0012] Furthermore, the non-oxidizing atmosphere includes any one or more of nitrogen, argon, and CO; the oxygen content in the non-oxidizing atmosphere is 8% to 18%.

[0013] Furthermore, the cooling is carried out at a rate of 2 to 5°C / min or cooled with the furnace to below 200°C and then taken out of the furnace.

[0014] Furthermore, the mold is any one of a graphite mold, a cast iron mold, and a stainless steel mold.

[0015] Advantages achieved by the present application compared with the prior art: (1) The method for preparing black microcrystalline glass from molten nickel-iron slag provided by the present application realizes the preparation of pure black microcrystalline glass through atmosphere control, has a simple process flow, and makes full use of the sensible heat of high-temperature slag; (2) In the steps of the method for preparing black microcrystalline glass, there is no need to perform iron reduction and addition of additional colorants, and color change will not occur during the preparation of black microcrystalline glass, effectively improving the purity of black microcrystalline glass; (3) Only a small amount of conditioning agent and nickel-iron slag are used to prepare black microcrystalline glass products, the formula composition is simple, the large-scale production cost is reduced, the utilization rate of nickel-iron slag reaches 70-95%, and the effective utilization of waste resources is realized; (4) The performance of the obtained black microcrystalline glass products is higher than the requirements of the microcrystalline glass building industry standard, and has better hardness, compressive strength, wear resistance, acid and alkali resistance and other properties, improving market competitiveness. Description of the Drawings

[0016] Figure 1 It is a process flow diagram of the method for preparing black microcrystalline glass from molten nickel-iron slag provided by the embodiment of the present application; Figure 2 It is a sample diagram of the black microcrystalline glass obtained in Example 1; Figure 3 It is an XRD diagram of the sample obtained in Example 1; Figure 4 It is a sample diagram of the black microcrystalline glass obtained in Example 2; Figure 5 It is a cross-sectional view of the sample obtained in Example 3; Figure 6 It is a cross-sectional view of the sample obtained in Example 4; Figure 7 It is a sample diagram of the black microcrystalline glass obtained in Example 5; Figure 8 It is an XRD diagram of the red part of the sample obtained in Example 5. Detailed Embodiments

[0017] The technical solution of the present application will be described in detail below through the drawings and specific embodiments. It should be understood that the specific features in the embodiments of the present application are a detailed description of the technical solution of the present application, rather than a limitation of the technical solution of the present application.

[0018] The present application provides a method for preparing black microcrystalline glass from molten nickel-iron slag, and the process flow is as Figure 1 shown, including: (1)Directly feed the high-temperature molten nickel-iron slag into a slag ladle at 1442°C to 1568°C, and add a conditioning agent; the content of nickel-iron slag is 70% to 95%, and the content of the conditioning agent is 5% to 30%. The conditioning agent is divided into composition adjustment raw materials and clarification raw materials. Among them, the mass of the composition adjustment raw materials is 98% to 100% of the mass of the conditioning agent, and the mass of the clarification raw materials is 0% to 2% of the mass of the conditioning agent. The composition adjustment raw materials are one or a mixture of limestone, quartz sand, borax, and bauxite powder. Among them, the clarification raw materials are one or a mixture of industrial-grade antimony oxide and industrial-grade sodium chloride. The specific addition amount of the composition adjustment raw materials needs to refer to the composition of the actual molten nickel-iron slag used, and it is sufficient to ensure that the homogenized melt is within the required range.

[0019] (2)After adding the conditioning agent, keep it warm at a temperature above 1442°C, preferably at 1442°C to 1568°C, and the holding time is 30 min to 150 min for homogenization.

[0020] (3)Pour the homogenized melt into a mold to obtain a formed sample; the melt viscosity during the casting process is 0.1 Pa·s to 2.2 Pa·s.

[0021] (4)Place the formed sample in a crystallization furnace and conduct crystallization treatment under atmosphere control throughout the process. The crystallization temperature is 800°C to 950°C, and the crystallization time is 5 min to 60 min; among them, the atmosphere control process controls the oxygen content by introducing a non-oxidizing atmosphere, and the regulated oxygen content is 8% to 18%; among them, the non-oxidizing atmosphere is any one or a combination of nitrogen, argon, and CO.

[0022] (5)After crystallization, cool it at a rate of 2°C / min to 5°C / min or cool it in the furnace until it is below 200°C and then take it out of the furnace to obtain black microcrystalline stone.

[0023] In specific embodiments, unless otherwise specified, except for the clearly pointed out differences, the experimental environments and parameter conditions of each group in the test are kept consistent.

[0024] In some embodiments of the present application, the molten nickel-iron slag includes: SiO2: 40% to 60%, MgO: 20% to 40%, Fe2O3: 1% to 10%, FeO: 1% to 5%, Al2O3: 2% to 8%, CaO: 0.1% to 5%, Cr2O3: 0.1% to 5%, MnO: 0.1% to 1%, Na2O and K2O: 0.01% to 0.5%, and the rest are impurities.

[0025] In some other embodiments of the present application, the composition of the molten nickel-iron slag is as follows: (1)SiO2: 44.25%, MgO: 33.21%, Fe2O3: 14.27%, FeO: 1.38%, Al2O3: 3.04%, CaO: 0.93%, Cr2O3: 1.20%, MnO: 0.71%, Na2O and K2O: 0.14%.

[0026] (2)SiO2: 47.52%, MgO: 34.25%, Fe2O3: 9.27%, FeO: 1.40%, Al2O3: 3.27%, CaO: 1.34%, Cr2O3: 1.25%, MnO: 0.54%, Na2O and K2O: 0.24%.

[0027] In some embodiments of the present application, the homogenized melt comprises: SiO2: 48% - 60%, MgO: 18% - 38%, Fe2O3: 4% - 13%, FeO: 1% - 5%, Al2O3: 4% - 11%, CaO: 0.5% - 6%, B2O3: 0% - 6%, Cr2O3: 0.1% - 5%, MnO: 0.1% - 1%, Na2O and K2O: 0.01% - 0.5%.

[0028] In specific embodiments, the composition of the homogenized melt comprises: (1)SiO2: 50.32%, MgO: 27.57%, Fe2O3: 10.44%, FeO: 1.21%, Al2O3: 4.11%, CaO: 0.82%, B2O3: 3.11%, Cr2O3: 1.05%, MnO: 0.62%, Na2O and K2O: 0.12%.

[0029] (2)SiO2: 45.14%, MgO: 32.54%, Fe2O3: 8.81%, FeO: 1.33%, Al2O3: 5.83%, CaO: 1.27%, Cr2O3: 1.19%, MnO: 0.51%, Na2O and K2O: 0.23%, B2O3: 0.83%.

[0030] (3)SiO2: 50.32%, MgO: 23.25%, Fe2O3: 9.99%, FeO: 1.07%, Al2O3: 4.11%, CaO: 1.20%, B2O3: 8.11%, Cr2O3: 0.84%, MnO: 0.50%, Na2O and K2O: 0.08%.

[0031] The following further describes a method for preparing black microcrystalline glass from molten nickel - iron slag based on atmosphere regulation provided by the present application.

[0032] Example 1:

[0033] This embodiment provides a method for preparing black microcrystalline glass from molten nickel-iron slag, and the specific process is as follows: (1) The raw materials mainly include molten nickel-iron slag and a conditioning agent. The nickel-iron slag accounts for 86% of the total mass percentage, and the conditioning agent accounts for 14% of the total mass percentage. The composition-adjusting raw materials in the conditioning agent are a mixture of limestone, bauxite powder, and borax, accounting for 13% of the total mass percentage; the clarifying raw material component is industrial-grade antimony oxide, accounting for 1% of the total mass percentage.

[0034] (2) The composition of the molten nickel-iron slag by mass percentage is: SiO2: 44.25%, MgO: 33.21%, Fe2O3: 14.27%, FeO: 1.38%, Al2O3: 3.04%, CaO: 0.93%, Cr2O3: 1.20%, MnO: 0.71%, Na2O and K2O: 0.14%.

[0035] (3) Directly add the molten nickel-iron slag to the slag ladle and add the conditioning agent, and keep it warm at 1550 °C for 120 min in total. The composition of the glass melt obtained after melting and homogenization by mass percentage is: SiO2: 50.32%, MgO: 27.57%, Fe2O3: 10.44%, FeO: 1.21%, Al2O3: 4.11%, CaO: 0.82%, B2O3: 3.11%, Cr2O3: 1.05%, MnO: 0.62%, Na2O and K2O: 0.12%.

[0036] (4) When the viscosity of the molten slag is 0.6 Pa·s, pour it into the mold.

[0037] (5) Send the formed product into the crystallization furnace, introduce CO. At this time, the oxygen content in the atmosphere is 14%, the nitrogen content is 52%, and the CO content is 33%, and carry out crystallization treatment. The crystallization temperature is 900 °C, and after keeping warm for 45 min, it is cooled with the furnace to obtain black microcrystalline glass.

[0038] (6) Cut and polish the microcrystalline glass sample to obtain a sample. The sample picture is as Figure 2 shown. The upper part of the attached drawing is the external view, and the lower part is the sectional view; it can be seen from Figure 2 that: the surface and the interior of the sample are black, the surface is bright, there are almost no pores inside, and the whole is relatively dense. At this time, the ratio of Fe 3+ :Fe 2+ is 1.5.

[0039] The XRD result of the sample is as Figure 3 shown. The main crystal phase is aegirine, and a large number of forsterite and low-iron forsterite phases also exist. The density of the sample is 3.42 g / cm -3, the compressive strength is 345 MPa, the flexural strength is 142 MPa, the wear rate is 1.2%, the water absorption rate is 0.018%, it has good acid and alkali resistance, and the performance indicators are excellent.

[0040] Example 2:

[0041] This example provides a method for preparing black microcrystalline glass from molten nickel-iron slag, and the specific process is as follows: (1) The raw materials mainly include molten nickel-iron slag and a conditioning agent. The nickel-iron slag accounts for 95% of the total mass percentage; the conditioning agent accounts for 5% of the total mass percentage. Among them, the composition adjustment raw materials are a mixture of bauxite powder and borax, accounting for 4% of the total mass percentage, and the clarification raw material component is industrial-grade antimony oxide, accounting for 1% of the total mass percentage.

[0042] (2) The composition of the molten nickel-iron slag by mass percentage is: SiO2: 47.52%, MgO: 34.25%, Fe2O3: 9.27%, FeO: 1.40%, Al2O3: 3.27%, CaO: 1.34%, Cr2O3: 1.25%, MnO: 0.54%, Na2O and K2O: 0.24%.

[0043] (3) The molten nickel-iron slag is directly added to the slag ladle, and the conditioning agent is added, and they are kept warm at 1568 °C for 150 min; the composition of the glass melt obtained after melting and homogenization by mass percentage is: SiO2: 45.14%, MgO: 32.54%, Fe2O3: 8.81%, FeO: 1.33%, Al2O3: 5.83%, CaO: 1.27%, Cr2O3: 1.19%, MnO: 0.51%, Na2O and K2O: 0.23%, B2O3: 0.83%.

[0044] (4) When the viscosity of the molten slag is 0.1 Pa·s, it is poured into a mold.

[0045] (5) The formed product is sent into a crystallization furnace, and CO is introduced. At this time, the oxygen content in the atmosphere is 18%, the nitrogen content is 50%, and the CO content is 32%. Crystallization treatment is carried out at a crystallization temperature of 950 °C. After holding for 60 min, it is cooled at a cooling rate of 5 °C / min to obtain black microcrystalline glass.

[0046] (6) The microcrystalline glass sample is cut and polished to obtain a sample. The sample picture is as Figure 4 shown. The upper half of the attached drawing is the appearance view, and the lower half is the sectional view; according to Figure 4 it can be seen that: the surface and the interior of the sample are black, the surface is bright, there are almost no pores inside, the whole is relatively dense, and the density is 3.38 g / cm -3, The compressive strength is 338 MPa, the flexural strength is 140 MPa, the wear rate is 1.2%, the water absorption rate is 0.021%, it has good acid and alkali resistance, and the performance indicators are excellent.

[0047] Example 3:

[0048] This example provides a method for preparing black microcrystalline glass from molten nickel-iron slag. The specific process is as follows: (1) The raw materials mainly include molten nickel-iron slag and a conditioning agent. The nickel-iron slag accounts for 70% of the total mass percentage; the conditioning agent accounts for 30% of the total mass percentage. Among them, the composition-adjusting raw materials are a mixture of quartz sand, limestone, bauxite powder, and borax, accounting for 28% of the total mass percentage; the clarifying raw material composition is industrial-grade antimony oxide, accounting for 2% of the total mass percentage.

[0049] (2) The composition of the molten nickel-iron slag by mass percentage is: SiO2: 44.25%, MgO: 33.21%, Fe2O3: 14.27%, FeO: 1.38%, Al2O3: 3.04%, CaO: 0.93%, Cr2O3: 1.20%, MnO: 0.71%, Na2O and K2O: 0.14%.

[0050] (3) Directly add the molten nickel-iron slag to the slag ladle, and add the conditioning agent. Keep it warm for 30 minutes at 1442 °C; the composition of the glass melt obtained after melting and homogenization by mass percentage is: SiO2: 50.32%, MgO: 23.25%, Fe2O3: 9.99%, FeO: 1.07%, Al2O3: 4.11%, CaO: 1.20%, B2O3: 8.11%, Cr2O3: 0.84%, MnO: 0.50%, Na2O and K2O: 0.08%.

[0051] (4) When the viscosity of the molten slag is 2.2 Pa·s, pour it into the mold.

[0052] (5) Send the formed product into the crystallization furnace, introduce CO. At this time, the oxygen content in the atmosphere is 8%, the nitrogen content is 54%, and the CO content is 38%. Carry out crystallization treatment. The crystallization temperature is 800 °C. After keeping it warm for 5 minutes, cool it at a cooling rate of 2 °C / min to obtain black microcrystalline glass.

[0053] (6) Cut and polish the microcrystalline glass sample to obtain a sample. The cross-section of the sample is as Figure 5 shown, Figure 5 showing that the interior of the sample is black, there are almost no pores, and it is relatively dense as a whole. The density of the sample is 3.22 g / cm -3 , The compressive strength is 310 MPa, the flexural strength is 113 MPa, the wear rate is 1.4%, the water absorption rate is 0.030%, it has good acid and alkali resistance, and the performance indicators are excellent.

[0054] Example 4:

[0055] This example provides a method for preparing black microcrystalline glass from molten nickel-iron slag. The specific process is as follows: (1) The raw materials mainly include molten nickel-iron slag and a conditioning agent. The nickel-iron slag accounts for 86% of the total mass percentage; the conditioning agent accounts for 14% of the total mass percentage. Among them, the composition-adjusting raw materials are a mixture of limestone, bauxite powder, and borax, accounting for 13% of the total mass percentage; the clarifying raw material is industrial-grade antimony oxide, accounting for 1% of the total mass percentage.

[0056] (2) The composition of the molten nickel-iron slag by mass percentage is: SiO2: 44.25%, MgO: 33.21%, Fe2O3: 14.27%, FeO: 1.38%, Al2O3: 3.04%, CaO: 0.93%, Cr2O3: 1.20%, MnO: 0.71%, Na2O and K2O: 0.14%.

[0057] (3) The molten nickel-iron slag is directly added to a slag ladle, and the conditioning agent is added. They are kept warm at 1550 °C for 120 min in total; the composition of the glass melt obtained after melting and homogenization by mass percentage is: SiO2: 50.32%, MgO: 27.57%, Fe2O3: 10.44%, FeO: 1.21%, Al2O3: 4.11%, CaO: 0.82%, B2O3: 3.11%, Cr2O3: 1.05%, MnO: 0.62%, Na2O and K2O: 0.12%.

[0058] (4) When the viscosity of the molten slag is 0.6 Pa·s, it is poured into a mold.

[0059] (5) The formed product is sent into a crystallization furnace, and nitrogen is introduced. At this time, the oxygen content in the atmosphere is 10%, and the nitrogen content is 89%. Crystallization treatment is carried out. The crystallization temperature is 900 °C. After holding for 60 min, it is cooled with the furnace to obtain black microcrystalline glass.

[0060] (6) The microcrystalline glass sample is cut and polished to obtain a sample. The sample cross-section is as Figure 6 shown, Figure 6 showing that the surface and interior of the sample are black, with almost no pores, and the whole is relatively dense. The sample density is 3.48 g / cm -3 , the compressive strength is 340 MPa, the flexural strength is 138 MPa, the wear rate is 1.3%, the water absorption rate is 0.015%, and it has good acid and alkali resistance, and excellent performance indicators.

[0061] Example 5:

[0062] This example is an atmosphere comparative example. The atmosphere control process in Example 1 is removed, and microcrystalline glass is prepared in an air atmosphere. The specific process is as follows: (1) The raw materials mainly include molten nickel-iron slag and conditioning agents. The nickel-iron slag accounts for 86% of the total mass percentage; the conditioning agents account for 14% of the total mass percentage, among which the composition-adjusting raw materials are a mixture of limestone, bauxite powder, and borax, accounting for 13% of the total mass percentage; the clarifying raw material is industrial-grade antimony oxide, accounting for 1% of the total mass percentage.

[0063] (2) The composition of the molten nickel-iron slag by mass percentage is: SiO2: 44.25%, MgO: 33.21%, Fe2O3: 14.27%, FeO: 1.38%, Al2O3: 3.04%, CaO: 0.93%, Cr2O3: 1.20%, MnO: 0.71%, Na2O and K2O: 0.14%.

[0064] (3) The molten nickel-iron slag is directly added to the slag ladle, and the conditioning agents are added, and they are kept warm at 1550 °C for 120 min in total; the composition of the glass melt obtained after melting and homogenization by mass percentage is: SiO2: 50.32%, MgO: 27.57%, Fe2O3: 10.44%, FeO: 1.21%, Al2O3: 4.11%, CaO: 0.82%, B2O3: 3.11%, Cr2O3: 1.05%, MnO: 0.62%, Na2O and K2O: 0.12%.

[0065] (4) When the viscosity of the molten slag is 0.6 Pa·s, it is poured into the mold.

[0066] (5) The formed product is sent into the crystallization furnace, and crystallization treatment is carried out in an air atmosphere. The crystallization temperature is 900 °C. After keeping warm for 60 min, it is cooled with the furnace to obtain black microcrystalline glass.

[0067] (6) The cast stone sample is cut and polished to obtain a sample. The sample picture is as Figure 7 shown. The upper half of the attached drawing is the appearance view, and the lower half is the sectional view; it can be seen from Figure 7 that: the interior of the sample appears black, but the surface has obvious color change, presenting red, which does not reach the black effect and cannot meet the process requirements. The ratio of Fe 3+ :Fe 2+ in the red part is 2.8, and the content of Fe 3+ increases significantly; The XRD result of the red part of the sample is as Figure 8 shown. The main crystal phase of the sample is forsterite, and there is a certain amount of fayalite at the same time, and there is no aegirine phase.

[0068] Example VI:

[0069] In this embodiment, 100% of molten nickel-iron slag is used to prepare black microcrystalline glass, and the conditioning agent in the first embodiment is removed to compare the role of the conditioning agent in this application. The specific process is as follows: (1) The raw material is molten nickel-iron slag, and the nickel-iron slag accounts for 100% of the total mass percentage.

[0070] (2) The composition of the molten nickel-iron slag by mass percentage is: SiO2: 44.25%, MgO: 33.21%, Fe2O3: 14.27%, FeO: 1.38%, Al2O3: 3.04%, CaO: 0.93%, Cr2O3: 1.20%, MnO: 0.71%, Na2O and K2O: 0.14%.

[0071] (3) The molten nickel-iron slag is directly added to the slag ladle and kept warm at 1550 °C for 120 min.

[0072] (4) The sample is melted and kept warm at a predetermined temperature, and the viscosity cannot reach the required range. When the viscosity of the molten slag is 2.5 Pa·s, it is poured into a mold.

[0073] (5) The formed product is sent into a crystallization furnace, and CO is introduced. At this time, the oxygen content in the atmosphere is 14%, the nitrogen content is 52%, and the CO content is 33%. Crystallization treatment is carried out at a crystallization temperature of 900 °C. After holding for 60 min, it is cooled with the furnace to obtain black microcrystalline glass.

[0074] (6) The microcrystalline glass sample is cut and polished to obtain a sample. The density of the sample is 2.30 g / cm -3 , the compressive strength is 125 MPa, the flexural strength is 76 MPa, the wear rate is 4.8%, the water absorption rate is 3.2%, and the acid and alkali resistance is relatively low, and the performance indexes are significantly poor.

[0075] The above are only the preferred embodiments of this application. It should be noted that for those of ordinary skill in the art, without departing from the technical principle of this application, several improvements and deformations can still be made, and these improvements and deformations should also be regarded as the protection scope of this application.

Claims

1. A method for preparing black microcrystalline glass from molten nickel-iron slag, characterized in that, Including: Mixing molten nickel-iron slag and a conditioning agent in a mass composition ratio of 7:3 to 19:1, and performing melting and heat preservation to obtain a homogenized melt; Casting the homogenized melt into a mold to obtain a formed sample; Performing crystallization treatment on the formed sample under the condition of a non-oxidizing atmosphere, and cooling to obtain a black microcrystalline stone.

2. The method according to claim 1, wherein The temperature range of the crystallization treatment is 800°C to 950°C, and the time is 5 minutes to 60 minutes.

3. The method according to claim 1, characterized in that, The temperature range of the melting and heat preservation is 1442°C to 1568°C, and the heat preservation time is 30 minutes to 150 minutes; During casting, the viscosity of the homogenized melt is 0.1 Pa·s to 2.2 Pa·s.

4. The method according to claim 1, characterized in that The molten nickel-iron slag includes the following chemical components in mass percentages: SiO2: 40% to 60%, MgO: 20% to 40%, Fe2O3: 1% to 10%, FeO: 1% to 5%, Al2O3: 2% to 8%, CaO: 0.1% to 5%, Cr2O3: 0.1% to 5%, MnO: 0.1% to 1%, Na2O and K2O: 0.01% to 0.5%.

5. The method according to claim 1, wherein The homogenized melt includes the following chemical components in mass percentages: SiO2: 48% to 60%, MgO: 18% to 38%, Fe2O3: 4% to 13%, FeO: 1% to 5%, Al2O3: 4% to 11%, CaO: 0.5% to 6%, B2O3: 0% to 6%, Cr2O3: 0.1% to 5%, MnO: 0.1% to 1%, Na2O and K2O: 0.01% to 0.5%.

6. The method according to claim 1, wherein The conditioning agent includes a composition adjusting raw material and a clarifying raw material; wherein the mass of the composition adjusting raw material is 98% to 100% of the mass of the conditioning agent, and the mass of the clarifying raw material is 0% to 2% of the mass of the conditioning agent.

7. The method according to claim 6, wherein The composition adjusting raw material is any one or more of limestone, quartz sand, borax, and bauxite powder; the clarifying raw material is a mixture of one or more of industrial-grade antimony oxide and industrial-grade sodium chloride.

8. The method according to claim 1, wherein The non-oxidizing atmosphere includes any one or more of nitrogen, argon, and CO; the oxygen content in the non-oxidizing atmosphere is 8% to 18%.

9. The method according to claim 1, characterized in that, The cooling is at a rate of 2°C / min to 5°C / min or cooling with the furnace to below 200°C and then discharging from the furnace.

10. The method according to claim 1, characterized in that, The mold is any one of a graphite mold, a cast iron mold, and a stainless steel mold.

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