CN120796719A - Recycling treatment method for waste refractory materials - Google Patents
Recycling treatment method for waste refractory materialsInfo
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- CN120796719A CN120796719A CN202511299863.8A CN202511299863A CN120796719A CN 120796719 A CN120796719 A CN 120796719A CN 202511299863 A CN202511299863 A CN 202511299863A CN 120796719 A CN120796719 A CN 120796719A
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Abstract
本发明涉及一种废旧耐火材料的资源化处理方法，包括如下步骤：将含有镁的氧化物和铬的氧化物的废旧耐火材料和足量的炭粉混合均匀后，压制成型，获得料块；将所述料块于真空或保护气氛条件下加热至温度T1，使得料块中的镁的氧化物与炭粉反应生成镁蒸气，反应完毕后，获得料块残留体；期间，收集镁蒸气，冷凝，获得金属镁；将料块残留体于真空条件下加热至温度T2，反应完毕后，冷却，获得粗铬；将所述粗铬破碎后，依次碱浸、水洗、酸浸、水洗、干燥，获得金属铬产品。本发明实现了废旧耐火材料中镁、铬的同时回收，效率高，且降低了生产能耗，反应过程既不产生废水，也无危害性废气产生。
The present invention relates to a method for recycling waste refractory materials, comprising the following steps: uniformly mixing waste refractory materials containing magnesium oxide and chromium oxide with a sufficient amount of carbon powder, and then pressing and forming the mixture to obtain a block; heating the block to a temperature T1 under vacuum or a protective atmosphere, so that the magnesium oxide in the block reacts with the carbon powder to generate magnesium vapor. After the reaction is complete, a block residue is obtained; during this process, the magnesium vapor is collected and condensed to obtain metallic magnesium; heating the block residue to a temperature T2 under vacuum, and after the reaction is complete, cooling to obtain crude chromium; crushing the crude chromium, and then sequentially alkali leaching, water washing, acid leaching, water washing, and drying to obtain a metallic chromium product. The present invention achieves the simultaneous recovery of magnesium and chromium from waste refractory materials, is highly efficient, and reduces production energy consumption. The reaction process produces neither wastewater nor hazardous exhaust gas.
Description
Technical Field
The invention relates to a recycling treatment method of waste refractory materials, and belongs to the technical field of general industrial solid waste recycling environment-friendly comprehensive utilization and metal smelting.
Background
The high temperature industries such as steel, cement, glass and the like and various industrial kilns consume a large amount of refractory materials, a large amount of waste refractory bricks containing magnesium and/or chromium, lining and other waste materials such as waste high-chromium bricks, magnesia-chrome bricks, chrome corundum and the like are generated, and in addition, magnesium and chrome refractory material production enterprises can generate a large amount of waste materials containing magnesium and/or chrome in the process of producing the refractory material products. The above waste materials and scraps may be collectively referred to as waste refractory materials. The waste refractory materials are huge in quantity and extremely difficult to process, and most of the waste refractory materials are typically processed in a buried or degraded mode except that few waste refractory materials can be returned to a production line for reuse. The accumulation or burial treatment needs to occupy land, increases cost, and also causes great waste of resources and serious environmental pollution risks.
The existing recovery process of waste refractory materials is mainly divided into a fire recovery process, a wet recovery process and the like, wherein the fire recovery process is high in energy consumption and low in chromium recovery rate, in addition, aiming at refractory materials containing magnesium and chromium at the same time, the difficult problem of separation of magnesium and chromium is solved, only single elements such as chromium can be recovered, a large amount of Cr 3+ -containing wastewater can be generated in the wet recovery process, even Cr 6+ wastewater can be generated, the wastewater treatment burden is high, the cost is high, and environmental pollution is easy to cause.
The Chinese patent application CN119824250A discloses a method for producing high-purity metal chromium from waste chromium-containing refractory materials by using a carbon reduction method, which comprises the following steps of collecting the waste chromium-containing refractory materials, crushing the waste chromium-containing refractory materials to a granularity of 0.1-1mm, carrying out magnetic separation and impurity removal to obtain chromium-containing enriched matters, carrying out acid leaching and impurity removal to obtain chromium-rich raw materials, preparing the chromium-rich raw materials, carbon powder, yttrium-stabilized zirconia and lanthanum oxyfluoride into a mixture, pressing the mixture into a ball, carrying out a two-stage heating reduction process to obtain a reaction product, cooling the reaction product to 800-1000 ℃, carrying out preliminary separation of a slag removing phase through gravity sedimentation, carrying out electroslag remelting refining treatment on the residual metal phase to obtain refined metal chromium, and cooling to complete recovery of the metal chromium. The patent can realize good recovery of chromium in the waste chromium-containing refractory, but does not consider recovery of magnesium (the content is up to 41.0-42.2%) in the waste chromium-containing refractory, and rare earth additives such as yttrium stabilized zirconia, lanthanum oxyfluoride (LaOF) and the like are required to be added to realize separation and recovery of chromium elements, so that the price of the rare earth elements is higher, the treatment cost is increased, and the risk of environmental pollution caused by fluoride and rare earth substances is increased.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a recycling treatment method of waste refractory materials so as to realize the recovery of magnesium and chromium in the waste refractory materials.
In order to solve the technical problems, the technical scheme of the invention is as follows:
A recycling treatment method of waste refractory materials comprises the following steps:
s1, providing powdery waste refractory materials;
Wherein the waste refractory material contains magnesium oxide and chromium oxide;
S2, uniformly mixing the waste refractory material with a sufficient amount of carbon powder, and then compacting to obtain a block;
S3, heating the material block to a temperature T1 under the condition of vacuum or protective atmosphere, so that magnesium oxide in the material block reacts with carbon powder to generate magnesium vapor, and obtaining a material block residual body after the reaction is finished;
during the period, collecting magnesium vapor, condensing to obtain magnesium metal;
S4, heating the material block residual body to a temperature T2 under the condition of vacuum or protective atmosphere, so that chromium oxide in the material block residual body reacts with carbon powder to generate metal chromium, and cooling after the reaction is finished to obtain crude chromium;
wherein T2 is more than T1, T2 is less than the melting point of metallic chromium, T1 is higher than the boiling point of metallic magnesium;
s5, crushing the crude chromium, and sequentially performing alkaline leaching, water washing, acid leaching, water washing and drying to obtain a metal chromium product.
The method comprises the steps of carrying out a two-step carbothermic reduction process, namely firstly reducing magnesium oxide in a waste refractory material under a lower temperature condition to generate magnesium vapor, separating magnesium element from other elements in the waste refractory material, and forming a certain pore in a block, wherein on one hand, in the carbothermic reduction process of the first section, the reaction consumption of magnesium oxide and carbon powder and the formation and escape of magnesium vapor are favorable for forming pores in the block, the discharge of gases such as magnesium vapor and CO 2 is promoted, the reaction of magnesium oxide and carbon powder is promoted (the reaction generated by the gases is promoted, the gas is timely discharged, the forward reaction is promoted), and on the other hand, the pores formed by the carbothermic reduction reaction of the first section can lead gases such as CO 2 generated in the carbothermic reduction reaction process of chromium oxide and carbon powder of the second section are timely discharged, the material is also favorable for being heated more uniformly, and the reaction of chromium oxide and carbon powder in residues is promoted, and the reaction rate of the residual is promoted. And removing impurities such as aluminum oxide, silicon oxide, unreacted magnesium oxide and the like through alkaline leaching and acid leaching, so as to obtain a metal chromium product with higher purity. Therefore, the invention can realize the recycling recovery of magnesium and chromium in the waste refractory material at the same time, does not need to be externally added with additives such as rare earth fluoride, and the like, and is beneficial to saving the cost and avoiding secondary pollution.
Further, in S1, the waste refractory material is the waste refractory material after magnetic separation to remove magnetic substances. Therefore, scrap materials such as scrap iron in waste refractory materials can be removed, subsequent treatment is facilitated, the collected magnetic scrap materials such as scrap iron can be further used for recycling iron, recycling utilization is realized, and treatment benefit is improved.
Further, in S1, the particle size of the waste refractory material is 100-200 meshes, and further 120-180 meshes.
Further, in S1, the content of the oxide containing magnesium in the waste refractory material is more than or equal to 50wt% calculated by MgO. The control of the content of a certain oxide containing magnesium is helpful for obtaining better chromium and magnesium recovery effect.
Further, in S1, the waste refractory material contains 52 to 90wt% of magnesium oxide, 55 to 85wt% of magnesium oxide, 60 to 80wt% of magnesium oxide, and 65 to 75wt% of magnesium oxide.
Further, in S1, the content of chromium-containing oxide in the waste refractory material is 5-45wt%, further 8-42wt%, further 12-38wt%, and further 16-32wt%, calculated as Cr 2O3.
Optionally, the content of alumina Al 2O3 in the waste refractory material is 1-3wt%, and the content of silica SiO 2 is 1-3wt%.
Alternatively, the waste refractory material is formed by combining two or more waste refractory materials, for example, one or more of high chrome brick, magnesia chrome brick and chrome corundum. Optionally, magnesia and/or chromia can be added to the waste refractory material as required to bring the content of magnesia and chromia in the raw material to the target value.
Further, in S2, the addition amount of the carbon powder is 1 to 3 times, more preferably 1.2 to 2.8 times, still more preferably 1.5 to 2.5 times of the theoretical amount of the carbon powder required for reducing all magnesium oxides and chromium oxides in the waste refractory material into metal magnesium and metal chromium through carbothermic reduction reaction.
Preferably, the purity of the carbon powder is more than or equal to 99.5 weight percent.
Optionally, the shape of the material block is one or more of cuboid, cube and cylinder.
Alternatively, the block is a cube with a side length of 80-120 mm.
Further, a plurality of uniformly distributed honeycomb holes are formed in the material block.
Further, in S2, the molding is performed by pressing under a pressure of 3-4 MPa.
Further, the temperature T1 is less than or equal to 1100 ℃ and less than or equal to 1200 ℃, and the temperature T2 is less than or equal to 1400 ℃ and less than or equal to 1500 ℃.
Still further, 1120 ℃ is less than or equal to T1 is less than or equal to 1180 ℃,1420 ℃ is less than or equal to T2 is less than or equal to 1480 ℃.
Still further, 1140 ℃ is less than or equal to T1 is less than or equal to 1160 ℃,1440 ℃ is less than or equal to T2 is less than or equal to 1460 ℃.
Preferably, in S3, the mass is heated to a temperature T1 under vacuum.
Alternatively, in S3, magnesium vapor may be collected by suction and sent to a condenser to be condensed to obtain magnesium metal.
Alternatively, the condensing temperature is 400-780 ℃, further 420-750 ℃.
Further, in S3, the reaction time is 5-7h, more preferably 5.5-6.5h, and in S4, the reaction time is 2-3h, more preferably 2.2-2.8h.
Preferably, in S4, the slug-residual mass is heated to a temperature T2 under vacuum conditions.
Alternatively, S3 and S4 are performed in a vacuum heating furnace.
Optionally, in S3 and S4, during the reaction, the pressure in the vacuum heating furnace is controlled to be 150Pa or less, and further 100Pa or less.
Further, in S4, cooling is performed with the furnace. Preferably, the furnace is cooled to below 100 ℃.
Further, in S5, after crushing the crude chromium, reacting in a sodium hydroxide solution at 80-100 ℃ for 2-4 hours, carrying out solid-liquid separation, washing the solid phase until washing water is neutral, then reacting in a sulfuric acid solution at 80-100 ℃ for 3-4 hours, carrying out solid-liquid separation, washing the solid phase until the washing water is neutral, and then drying for 10-14 hours at 80-100 ℃ to obtain a metal chromium product, wherein the concentration of the sodium hydroxide solution is 15-40wt%, further 20-30wt% and the concentration of the sulfuric acid solution is 5-10wt%.
Further, in S5, the crude chromium is crushed to 100-200 mesh.
Compared with the prior art, the invention has the following beneficial effects:
(1) The invention realizes simultaneous recovery of magnesium and chromium in waste refractory materials, has high efficiency, reduces production energy consumption, and does not produce waste water or harmful waste gas in the reaction process.
(2) The invention can realize the effective recovery of magnesium and chromium, and the product purity of the metal magnesium and the metal chromium is higher, the economic value is higher, the purity of the metal magnesium can reach 98wt%, the recovery rate of the magnesium can reach more than 80wt%, the purity of the metal chromium can reach more than 97wt%, and the recovery rate of the chromium can reach more than 79 wt%.
(3) The invention does not need to add rare earth additives such as yttrium stabilized zirconia, lanthanum oxyfluoride and the like, and is beneficial to reducing the cost and the post-treatment burden.
(4) The recycling treatment method of the waste refractory material can effectively consume the waste refractory material, realize recycling recovery of elements such as magnesium, chromium and the like, and effectively reduce the landfill pressure of the waste refractory material, and the potential safety hazard brought by adding the waste refractory material as recycled aggregate into a newly manufactured refractory material to a high-temperature high-pressure kiln.
Drawings
FIG. 1 is a flow chart of a method for recycling waste refractory material according to the present invention.
Detailed Description
The present invention will be described in detail with reference to examples. It should be noted that, without conflict, the embodiments of the present invention and features of the embodiments may be combined with each other. The relevant percentages refer to mass percentages unless otherwise indicated.
Example 1
The recycling treatment method of the waste refractory material comprises the following steps:
(1) Crushing and deironing, namely crushing the waste magnesia-chrome bricks to 100 meshes, and removing magnetic substances such as iron and the like in the waste magnesia-chrome bricks by magnetic separation to obtain magnesia-chrome brick powder (namely waste refractory material powder, wherein the MgO content is 60 percent and the Cr 2O3 content is 20 percent);
(2) Weighing 100kg of waste refractory material powder, weighing corresponding carbon powder according to a carbon distribution coefficient (namely, the theoretical quantity of the carbon powder required by reducing all MgO and Cr 2O3 in the waste refractory material powder into metal magnesium and metal chromium through carbothermic reduction reaction, which is the same as the theoretical quantity of the carbon powder), uniformly mixing the waste refractory material powder and the carbon powder, and pressing into square blocks with the side length of 100mm by using the pressure of 3.4MPa (wherein 36 honeycomb holes with the diameter of 8mm are uniformly distributed in the square blocks) so as to better ensure good air permeability and reaction activity;
(3) Placing a cube block in a vacuum heating furnace, closing a furnace door, vacuumizing, heating to 1150 ℃ under vacuum condition, preserving heat and reacting for 6 hours to enable magnesium oxide and carbon powder to react to generate magnesium vapor, collecting the magnesium vapor during the reaction, then heating to 1450 ℃, preserving heat and reacting for 2.5 hours to enable chromium oxide and carbon powder to react to generate metal chromium, cooling to 100 ℃ along with the furnace after the reaction is finished, and opening the furnace door to obtain crude chromium;
Controlling the pressure in the vacuum heating furnace to be less than or equal to 100Pa during the reaction;
feeding magnesium vapor into a condenser for condensation to obtain magnesium metal, wherein the condensation temperature is controlled to be less than or equal to 750 ℃ during the condensation period;
(4) The method comprises the steps of removing impurities, crushing crude chromium to 100 meshes, placing the crushed crude chromium in a 20 wt% sodium hydroxide solution with the concentration of 80 ℃ for reaction for 2 hours, filtering to obtain a solid phase 1, washing the solid phase 1 by deionized water until washing water is neutral, filtering to obtain a solid phase 2, placing the solid phase 2 in a 90 ℃ sulfuric acid solution with the concentration of 8wt% for reaction for 3.5 hours, filtering to obtain a solid phase 3, washing the solid phase 3 by deionized water until washing water is neutral, filtering to obtain a solid phase 4, and drying the solid phase 4 at 80 ℃ for 12 hours to obtain a metal chromium product.
The quality of the metal magnesium is detected to be 30.4kg, the purity of the magnesium is 89.92%, the recovery rate of the magnesium is 75.94%, the quality of the metal chromium product is 11.57kg, the purity of the chromium is 88.16%, and the recovery rate of the chromium is 74.56%. The purity was obtained by inductively coupled plasma emission spectrometry (ICP-OES) detection, as follows.
Example 2
Example 1 was repeated except that in step (1), the mass fraction of MgO in the waste refractory powder was 62.5% and the mass fraction of Cr 2O3 was 16%. Specifically, the waste refractory material powder consists of magnesia chrome brick powder 1 (MgO content 60%, cr 2O3 content 20%) and magnesia chrome brick powder 2 (MgO content 65%, cr 2O3 content 12%) according to a mass ratio of 1:1 (namely, consists of two waste magnesia chrome brick powders with different magnesium oxide and chromium oxide contents).
The quality of the metal magnesium is 32.21kg, the purity of the magnesium is 90.14%, the recovery rate of the magnesium is 77.43%, the quality of the metal chromium product is 9.11kg, the purity of the chromium is 90.02%, and the recovery rate of the chromium is 76.32%.
Example 3
Example 1 was repeated except that in step (1), the mass fraction of MgO in the spent refractory powder was 67.5% and the mass fraction of Cr 2O3 was 14%. Specifically, the waste refractory material powder consists of magnesia-chrome brick powder 1 (MgO content 60%, cr 2O3% and 20%) and magnesia-chrome brick powder 2 (MgO content 75%, cr 2O3% and 8%) according to a mass ratio of 1:1.
The quality of the metal magnesium is 33.26kg, the purity of the magnesium is 95.76%, the recovery rate of the magnesium is 78.64%, the quality of the metal chromium product is 7.86kg, the purity of the chromium is 93.2%, and the recovery rate of the chromium is 76.5%.
Example 4
Example 1 was repeated except that in step (1), the mass fraction of MgO in the waste refractory powder was 70% and the mass fraction of Cr 2O3 was 13%. Specifically, the waste refractory material powder consists of magnesia-chrome brick powder 1 (MgO content 60%, cr 2O3 content 20%) and magnesia-chrome brick powder 2 (MgO content 80%, cr 2O3 content 6%) according to a mass ratio of 1:1.
The quality of the metal magnesium is 34.89kg, the purity of the magnesium is 97.24%, the recovery rate of the magnesium is 80.78%, the quality of the metal chromium product is 7.18kg, the purity of the chromium is 97.98%, and the recovery rate of the chromium is 79.14%. The porosity of the material after the reaction of the magnesium metal is calculated to be 60.02 percent.
Example 5
Example 1 was repeated except that in step (1), the waste refractory powder (magnesia-chrome brick powder) had an MgO content of 80% and a Cr 2O3 content of 6%.
The quality of the metal magnesium is detected to be 40.14kg, the purity of the magnesium is 98%, the recovery rate of the magnesium is 81.96%, the quality of the metal chromium product is detected to be 3.15kg, the purity of the chromium is 94.48%, and the recovery rate of the chromium is 72.46%.
Example 6
Example 1 was repeated except that in step (1), the mass fraction of MgO in the waste refractory powder was 66% and the mass fraction of Cr 2O3 was 13%, specifically, the waste refractory powder consisted of magnesia-chromite brick powder 1 (MgO content 60%, cr 2O3 content 16%) and magnesia-chromite brick powder 2 (MgO content 80%, cr 2O3 content 6%) in a mass ratio of 7:3.
The detection shows that the mass of the metal magnesium block is 32.37kg, the purity of the magnesium is 95.96%, the recovery rate of the magnesium is 78.45%, the mass of the metal chromium product is 7.01kg, the purity of the chromium is 96.98%, and the recovery rate of the chromium is 76.43%.
Example 7
Example 2 was repeated except that in step (1), the mass fraction of MgO in the waste refractory material powder was 52.5% and the mass fraction of Cr 2O3 was 16%, specifically, the waste refractory material consisted of magnesia-chromite brick powder 1 (MgO content 40%, cr 2O3 content 20%) and magnesia-chromite brick powder 2 (MgO content 65%, cr 2O3 content 12%) in a mass ratio of 1:1.
The quality of the metal magnesium is 25.95kg, the purity of the magnesium is 86.45%, the recovery rate of the magnesium is 71.23%, the quality of the metal chromium product is 8.77kg, the purity of the chromium is 87.02%, and the recovery rate of the chromium is 70.98%.
Example 8
Example 2 was repeated except that in step (1), the waste refractory powder (magnesia-chrome brick powder) had a MgO content of 45% and a Cr 2O3 content of 16%.
The quality of the metal magnesium is 22.75kg, the purity of the magnesium is 83.23%, the recovery rate of the magnesium is 70.13%, the quality of the metal chromium product is 9.08kg, the purity of the chromium is 80.78%, and the recovery rate of the chromium is 68.23%.
By contrast, the control of the MgO content in the waste refractory powder within a specific range is helpful to obtain particularly excellent recovery rate and purity index of magnesium metal and chromium metal, and further particularly excellent recovery benefit is obtained. The possible reasons are that the content of MgO in the waste refractory powder affects the porosity or porosity of the residual material of the block after carbothermic reduction, and further affects the carbothermic reduction reaction process of chromium oxide, particularly, when the content of MgO in the waste refractory powder is low, the porosity of the pores of the residual material of the block is low, the gas generated by the carbothermic reduction reaction of chromium oxide is difficult to timely discharge, and the heat transfer is weak, which is unfavorable for the generation of chromium metal, and results in lower recovery rate of chromium metal and lower purity of chromium.
The foregoing examples are set forth in order to provide a more thorough description of the present application and are not intended to limit the scope of the application, and various modifications of the application, which are equivalent to those skilled in the art upon reading the present application, will fall within the scope of the application as defined in the appended claims.
Claims (10)
1. A recycling treatment method of waste refractory materials is characterized by comprising the following steps:
s1, providing powdery waste refractory materials;
Wherein the waste refractory material contains magnesium oxide and chromium oxide;
S2, uniformly mixing the waste refractory material with a sufficient amount of carbon powder, and then compacting to obtain a block;
S3, heating the material block to a temperature T1 under the condition of vacuum or protective atmosphere, so that magnesium oxide in the material block reacts with carbon powder to generate magnesium vapor, and obtaining a material block residual body after the reaction is finished;
during the period, collecting magnesium vapor, condensing to obtain magnesium metal;
S4, heating the material block residual body to a temperature T2 under the condition of vacuum or protective atmosphere, so that chromium oxide in the material block residual body reacts with carbon powder to generate metal chromium, and cooling after the reaction is finished to obtain crude chromium;
wherein T2 is more than T1, T2 is less than the melting point of metallic chromium, T1 is higher than the boiling point of metallic magnesium;
s5, crushing the crude chromium, and sequentially performing alkaline leaching, water washing, acid leaching, water washing and drying to obtain a metal chromium product.
2. The recycling method according to claim 1, wherein in S1, the waste refractory material is a waste refractory material from which magnetic substances are removed by magnetic separation.
3. The recycling method according to claim 1, wherein in S1, the content of magnesium-containing oxide in the waste refractory is not less than 50% by weight in terms of MgO.
4. The recycling method according to claim 2, wherein in S1, the content of the oxide containing magnesium in terms of MgO in the waste refractory is 52 to 90wt%.
5. The recycling method according to claim 1, wherein in S1, the content of chromium-containing oxides in the waste refractory is 5 to 45wt% in terms of Cr 2O3.
6. The recycling treatment method according to any one of claims 1 to 5, characterized in that in S2, the addition amount of the carbon powder is 1 to 3 times the theoretical amount of the carbon powder required for reducing all the magnesium oxide and chromium oxide in the waste refractory material to metallic magnesium and metallic chromium by carbothermic reduction reaction.
7. The recycling method according to any one of claims 1 to 5, wherein a plurality of uniformly distributed honeycomb cells are formed in the block.
8. The recycling treatment method according to any one of claims 1 to 5, wherein 1100 ℃ or less T1 or less 1200 ℃,1400 ℃ or less T2 or less 1500 ℃.
9. The recycling method according to any one of claims 1 to 5, wherein in S3, the reaction time is 5 to 7 hours, and in S4, the reaction time is 2 to 3 hours.
10. The recycling method according to any one of claims 1 to 5, wherein in S5, after the coarse chromium is crushed, the coarse chromium is reacted in a sodium hydroxide solution at 80 to 100 ℃ for 2 to 4 hours and then subjected to solid-liquid separation, the solid phase is washed with water until washing water is neutral, and after the coarse chromium is reacted in a sulfuric acid solution at 80 to 100 ℃ for 3 to 4 hours and then subjected to solid-liquid separation, the solid phase is washed with water until washing water is neutral and then dried for 10 to 14 hours at 80 to 100 ℃ to obtain a metal chromium product, wherein the concentration of the sodium hydroxide solution is 15 to 40wt% and the concentration of the sulfuric acid solution is 5 to 10wt%.
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