CN110117745B - Method for preparing ferrophosphorus alloy by adopting middle-low grade phosphorite and copper slag - Google Patents
Method for preparing ferrophosphorus alloy by adopting middle-low grade phosphorite and copper slag Download PDFInfo
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- CN110117745B CN110117745B CN201910463659.3A CN201910463659A CN110117745B CN 110117745 B CN110117745 B CN 110117745B CN 201910463659 A CN201910463659 A CN 201910463659A CN 110117745 B CN110117745 B CN 110117745B
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B5/00—General methods of reducing to metals
- C22B5/02—Dry methods smelting of sulfides or formation of mattes
- C22B5/10—Dry methods smelting of sulfides or formation of mattes by solid carbonaceous reducing agents
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C33/00—Making ferrous alloys
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/002—Ferrous alloys, e.g. steel alloys containing In, Mg, or other elements not provided for in one single group C22C38/001 - C22C38/60
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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- Y02P10/20—Recycling
Abstract
The invention discloses a method for preparing a ferro-phosphorus alloy by adopting middle-low grade phosphorite and copper slag, which comprises the following steps: firstly, respectively ball-milling middle-low grade phosphorite and copper slag by adopting a ball mill, then uniformly mixing the medium-low grade phosphorite and copper slag with a reducing agent, an additive and water, firstly sending the mixture into a mould for press forming under the argon atmosphere, then sending the mixture into a drying box for drying treatment until the water content is 0, finally sending the mixture into a resistance furnace for roasting, melting and removing residues to obtain a ferro-phosphorus alloy, and simultaneously taking the produced residues as raw materials for preparing cement. The invention comprehensively recycles the accumulated copper slag and the medium and low grade phosphorus ores which are not processed in large quantity, prepares the ferrophosphorus alloy with high added value, changes waste into valuable, improves the resource utilization rate, solves the problems in the prior art, and effectively solves the problems of higher cost, heavy pollution, high energy consumption and large output of three wastes when the medium and low grade phosphorus ores and copper slag are processed in the prior art.
Description
Technical Field
The invention belongs to the technical field of energy conservation, environmental protection and comprehensive utilization of resources, and particularly relates to a method for preparing a ferro-phosphorus alloy by adopting middle-low grade phosphorite and copper slag.
Background
The ferrophosphorus is an intermetallic compound with better mixing of iron and phosphorus, has good conductivity, higher density, stable chemical property at normal temperature and corrosion resistance, and is widely applied to the preparation of high-purity FePO4Synthetic spherical LiFePO4Preparing trisodium phosphate and iron oxide red products, preparing ferrophosphorus powder and the like. The ferrophosphorus alloy is an important raw material in the metallurgy and chemical industry, and has wide application. In the metallurgical industry, ferrophosphorus is mainly used as an alloy additive to accurately adjust the content of phosphorus in metal to any required level, and ferrophosphorus can also play a role of a deoxidizer in the smelting process; in the chemical industry, ferrophosphorus is mainly used for synthesizing phosphoric acid, phosphate, novel sound insulation materials, antirust coatings and the like. At present, ferro-phosphorus is mainly obtained from chemical by-products such as ferro-phosphorus ore, thermal phosphoric acid or calcium magnesium phosphate fertilizer. But due to the overuse of the ferro-phosphorus ore resource and the high energy consumption of the thermalized phosphoric acid, the quality of the phosphorite is improvedThe defects of high requirement, high cost and the like limit the development and application of the ferrophosphorus, so a novel low-cost ferrophosphorus production process is urgently needed.
The steel industry in China develops at a high speed, but high-quality iron ore resources are less and less, so that the resources are reasonably and fully utilized, the pressure of iron ore import is relieved, and the method becomes an important problem to be solved by Chinese steel enterprises. Copper is an indispensable important nonferrous metal in the fields of electricity, light industry, mechanical manufacturing, building, national defense and the like, and about 97 percent of copper in China is smelted from copper concentrate by a pyrogenic process. Reckoning according to 844 ten thousand of refined copper yield in 2016, and nearly 2000 ten thousand of copper slag produced every year. In the huge amount of copper slag, only a small amount of valuable elements are recycled, and the rest are stockpiled and processed. According to statistics, copper slag with the quantity of more than 1.4 hundred million t is piled up nationwide, and becomes industrial solid waste with a large quantity generated in the metallurgical industry. The copper slag is the metallurgical slag discharged from a copper smelting furnace in the pyrometallurgical copper smelting process, is a glass phase formed by cooling the upper layer of a molten material in the copper smelting furnace, mainly contains various valuable metals such as Fe, Cu, Zn, Pb, Co, Ni and the like and a small amount of noble metals such as Au, Ag and the like, wherein the main minerals are iron silicate and magnetic iron oxide, the grade of iron is generally over 40 percent and is far higher than the average industrial grade of 29.1 percent of iron ore, but the utilization rate of iron in the copper slag is less than 1 percent. Most of copper slag is piled up in a slag field, and can pollute surrounding water and soil, so that the environmental hazard is caused, and the waste of resources is also huge. Therefore, the strengthening of the harmless treatment of the copper slag resources is significant and imperative, and particularly, the recycling of the iron resources in the copper slag has certain economic benefits.
China has abundant phosphorite resources, the storage capacity of which is 193.6 hundred million tons and accounts for about 30 percent of the storage capacity of the phosphorite resources in the world, but the phosphorite resources are less in rich ore and more in lean ore, the average grade is only 17 percent, and the phosphorite (P) with medium and low grade cannot be directly utilized2O5<26%) accounts for more than 90%, and is one of countries with the lowest average grade of phosphate ores in the world. The development and utilization of phosphorite resources mainly take rich ore as a main part, and some high-quality phosphorite resources are not protectively exploited and scientifically and reasonably utilized, so that the high-quality phosphorite resources in Guizhou are seriously lost. In addition, the three wastes at the end of phosphorus chemical industryThe treatment difficulty is high, the comprehensive utilization of phosphorite resources is insufficient, and the technical innovation needs to be enhanced urgently. At present, rich ores are gradually exhausted, and researchers have to direct attention to phosphorite with lower grade. Based on this, how to fully utilize the medium-low grade phosphorite and improve the comprehensive utilization rate and the economic benefit of the phosphorite is of great importance.
Currently, there are some documents on the preparation of gold-iron alloys, such as:
1. patent application CN201310123248.2 discloses a method for preparing a phosphorus-iron alloy by using high-phosphorus iron ore and medium and low grade phosphate ore, which comprises the steps of mixing high-phosphorus oolitic hematite and medium and low grade phosphate ore which are crushed to minus 3mm in advance according to a certain proportion, agglomerating, reducing and roasting the dried agglomerates by using coal as a reducing agent, wherein the roasting temperature is 1150-1200 ℃, the roasting time is 90-120 min, and grinding and selecting the cooled reduced agglomerates to obtain a phosphorus-iron alloy product. The method directly prepares the ferro-phosphorus alloy by taking the poor oolitic hematite and medium and low grade phosphorite resources which are not effectively utilized in the 'dull' state at present as raw materials, and has the advantages of short process flow, low cost, high product added value and wide application prospect. The invention is easy to realize industrialization.
2. Patent application CN201310332335.9 discloses a preparation method of ferrophosphorus, wherein the weight ratio is 70-85%: 10-25%: 5-20% of the ferro-phosphorus slag, the high ferro-phosphorus ore and the dolomite are placed in a smelting furnace for smelting to obtain ferro-phosphorus. The preparation method of the ferrophosphorus has simple process, the utilization rate of the ferrophosphorus slag is up to more than 98 percent, so that the waste ferrophosphorus slag is recycled, the pollution to the environment is reduced, and the grade of the ferrophosphorus is improved. The invention also discloses ferrophosphorus prepared by the preparation method.
However, no relevant documents disclose that the middle-low grade phosphorite and the copper slag are made into the ferrophosphorus alloy, so that how to develop a novel low-cost and full-utilization middle-low grade phosphorite and copper slag and improve the comprehensive utilization rate and the economic benefit of the phosphorite and the copper slag is of great importance.
Disclosure of Invention
The invention provides a method for preparing a ferro-phosphorus alloy by adopting middle-low grade phosphorite and copper slag to solve the technical problems.
In order to achieve the above purpose, the invention adopts the following technical scheme:
a method for preparing a ferrophosphorus alloy by adopting middle-low grade phosphorite and copper slag comprises the following steps: firstly, respectively ball-milling the middle-low grade phosphorite and the copper slag by adopting a ball mill, then uniformly mixing the medium-low grade phosphorite and the copper slag with a reducing agent, an additive and water, firstly sending the mixture into a mould for compression molding under the argon atmosphere, then sending the mixture into a drying box for drying treatment until the water content is 0, and finally sending the mixture into a resistance furnace for roasting, and removing residues by melting to obtain the ferrophosphorus alloy.
The residue removed after melting can be used as raw material for preparing cement.
Further, the medium and low grade phosphorite, the copper slag, the reducing agent, the additive and the water are mixed according to the following weight part ratio: 25-35 parts of phosphorite, 60-80 parts of copper slag, 15-17 parts of reducing agent, 4-7 parts of additive and 0.4-0.7 part of water.
Further, the ball milling is to grind the materials into powder with the granularity of 80-120 meshes.
Further, the diameter of the die is 20.01-30 mm.
Further, the pressure of the compression molding is 12-18 MPa.
Further, the roasting temperature is 1200-1300 ℃, and the roasting time is 60-90 min.
Further, the drying temperature is not less than 120 ℃, and the drying time is 2-3 hours.
Further, the following steps: the reducing agent is coke powder.
Further, the additive is borax.
Further, the water is distilled water, deionized water or ultrapure water.
Due to the adoption of the technical scheme, the invention has the following beneficial effects:
(1) the invention takes the copper slag resources and the middle-low grade phosphate ores which are not processed and accumulated in large quantity at present as raw materials to prepare the ferrophosphorus alloy material with high added value, and provides a new thought and a new method for the comprehensive utilization of the complex and intractable copper slag and ore resources.
(2) The impurity content of the ferrophosphorus alloy is reduced in the treatment process, and the additive is added, so that the reducibility of the copper slag can be effectively improved, the growth of iron crystal grains is promoted, the reduction temperature is reduced, the cost is reduced, the energy consumption is reduced, and the discharge amount of three wastes is reduced; in addition, the additive used in the invention has wide sources and low cost, is easy to realize industrialized large-scale production, and is particularly suitable for the application of undeveloped medium-low grade phosphorite and copper slag resources.
(3) The method provided by the invention comprehensively recycles the medium-low grade phosphorite and the copper slag, changes waste into valuable, improves the resource utilization rate, solves the problems provided by the application, and effectively solves the problems of higher cost, heavy pollution, high energy consumption and large three-waste output when the medium-low grade phosphorite and the copper slag are treated in the prior art.
(4) The method has the advantages of low energy consumption, short process flow, high added value of products and wide application prospect, and can better realize the comprehensive utilization of medium and low grade phosphorite and copper slag.
Detailed Description
The following is a detailed description of the embodiments of the present invention, but the present invention is not limited to these embodiments, and any modifications or substitutions in the basic spirit of the embodiments are included in the scope of the present invention as claimed in the claims.
The copper slag used in the embodiment of the application is from a certain enterprise in Shandong province, the middle-low grade phosphate ore is from a certain enterprise in Guizhou province, the chemical components of the copper slag and the middle-low grade phosphorus are respectively analyzed, the mass fractions of the chemical components of the copper slag are shown in the following table 1, and the mass fractions of the chemical components of the middle-low grade phosphorus are shown in the following table 2.
TABLE 1 chemical composition and content of copper slag
TABLE 2 chemical composition and content of low-grade phosphorus ore
| Composition (I) | P2O5 | CaO | Fe2O3 | SiO2 | F | SiO3 | Al2O3 |
| Content (wt%) | 29 | 49 | 2 | 5 | 1.4 | 1.1 | 1 |
Example 1
A method for preparing a ferrophosphorus alloy by adopting middle-low grade phosphorite and copper slag comprises the following steps: firstly, respectively ball-milling middle-low grade phosphorite and copper slag by adopting a ball mill, then uniformly mixing the medium-low grade phosphorite and copper slag with a reducing agent, an additive and water, firstly sending the mixture into a mould for press forming under the argon atmosphere, then sending the mixture into a drying box for drying treatment until the water content is 0, finally sending the mixture into a resistance furnace for roasting, melting and removing residues to obtain a ferro-phosphorus alloy, and simultaneously taking the produced residues as raw materials for preparing cement.
Further, the medium and low grade phosphorite, the copper slag, the reducing agent, the additive and the water are mixed according to the following weight part ratio: 25 parts of phosphorite, 60 parts of copper slag, 15 parts of reducing agent, 4 parts of additive and 0.4 part of water; the ball milling is to grind the materials into powder with the granularity of 80 meshes; the diameter of the die is 20.01 mm; the pressure of the compression molding is 12 MPa; the roasting temperature is 1200 ℃, and the roasting time is 60 min; the drying temperature is more than or equal to 120 ℃, and the drying time is 2 hours; the reducing agent is coke powder; the additive is borax; the water is distilled water.
Example 2
A method for preparing a ferrophosphorus alloy by adopting middle-low grade phosphorite and copper slag comprises the following steps: firstly, respectively ball-milling middle-low grade phosphorite and copper slag by adopting a ball mill, then uniformly mixing the medium-low grade phosphorite and copper slag with a reducing agent, an additive and water, firstly sending the mixture into a mould for press forming under the argon atmosphere, then sending the mixture into a drying box for drying treatment until the water content is 0, finally sending the mixture into a resistance furnace for roasting, melting and removing residues to obtain a ferro-phosphorus alloy, and simultaneously taking the produced residues as raw materials for preparing cement.
Further, the medium and low grade phosphorite, the copper slag, the reducing agent, the additive and the water are mixed according to the following weight part ratio: 35 parts of phosphorite, 80 parts of copper slag, 17 parts of reducing agent, 7 parts of additive and 0.7 part of water; the ball milling is to grind the materials into powder with the granularity of 120 meshes; the diameter of the die is 30 mm; the pressure of the compression molding is 18 MPa; the roasting temperature is 1300 ℃, and the roasting time is 90 min; the drying temperature is more than or equal to 120 ℃, and the drying time is 3 hours; the reducing agent is coke powder; the additive is borax; the water is deionized water.
Example 3
A method for preparing a ferrophosphorus alloy by adopting middle-low grade phosphorite and copper slag comprises the following steps: firstly, respectively ball-milling middle-low grade phosphorite and copper slag by adopting a ball mill, then uniformly mixing the medium-low grade phosphorite and copper slag with a reducing agent, an additive and water, firstly sending the mixture into a mould for press forming under the argon atmosphere, then sending the mixture into a drying box for drying treatment until the water content is 0, finally sending the mixture into a resistance furnace for roasting, melting and removing residues to obtain a ferro-phosphorus alloy, and simultaneously taking the produced residues as raw materials for preparing cement.
Further, the medium and low grade phosphorite, the copper slag, the reducing agent, the additive and the water are mixed according to the following weight part ratio: 27 parts of phosphorite, 65 parts of copper slag, 15.5 parts of reducing agent, 5 parts of additive and 0.5 part of water; the ball milling is to grind the materials into powder with the granularity of 80-120 meshes; the diameter of the die is 22 mm; the pressure of the compression molding is 13 MPa; the roasting temperature is 1220 ℃, and the roasting time is 70 min; the drying temperature is more than or equal to 120 ℃, and the drying time is 2.2 h; the reducing agent is coke powder; the additive is borax; the water is distilled water, deionized water or ultrapure water.
Example 4
A method for preparing a ferrophosphorus alloy by adopting middle-low grade phosphorite and copper slag comprises the following steps: firstly, respectively ball-milling middle-low grade phosphorite and copper slag by adopting a ball mill, then uniformly mixing the medium-low grade phosphorite and copper slag with a reducing agent, an additive and water, firstly sending the mixture into a mould for press forming under the argon atmosphere, then sending the mixture into a drying box for drying treatment until the water content is 0, finally sending the mixture into a resistance furnace for roasting, melting and removing residues to obtain a ferro-phosphorus alloy, and simultaneously taking the produced residues as raw materials for preparing cement.
Further, the medium and low grade phosphorite, the copper slag, the reducing agent, the additive and the water are mixed according to the following weight part ratio: 33 parts of phosphorite, 75 parts of copper slag, 16.5 parts of reducing agent, 6 parts of additive and 0.6 part of water; the ball milling is to grind the materials into powder with the granularity of 110 meshes; the diameter of the die is 28 mm; the pressure of the compression molding is 17 MPa; the roasting temperature is 1280 ℃, and the roasting time is 80 min; the drying temperature is more than or equal to 120 ℃, and the drying time is 2.8 h; the reducing agent is coke powder; the additive is borax; the water is distilled water, deionized water or ultrapure water.
Example 5
A method for preparing a ferrophosphorus alloy by adopting middle-low grade phosphorite and copper slag comprises the following steps: firstly, respectively ball-milling middle-low grade phosphorite and copper slag by adopting a ball mill, then uniformly mixing the medium-low grade phosphorite and copper slag with a reducing agent, an additive and water, firstly sending the mixture into a mould for press forming under the argon atmosphere, then sending the mixture into a drying box for drying treatment until the water content is 0, finally sending the mixture into a resistance furnace for roasting, melting and removing residues to obtain a ferro-phosphorus alloy, and simultaneously taking the produced residues as raw materials for preparing cement.
Further, the medium and low grade phosphorite, the copper slag, the reducing agent, the additive and the water are mixed according to the following weight part ratio: 30 parts of phosphorite, 70 parts of copper slag, 16 parts of reducing agent, 5.5 parts of additive and 0.55 part of water; the ball milling is to grind the materials into powder with the granularity of 100 meshes; the diameter of the die is 25 mm; the pressure of the compression molding is 15 MPa; the roasting temperature is 1200-1300 ℃, and the roasting time is 75 min; the drying temperature is more than or equal to 120 ℃, and the drying time is 2.5 h; the reducing agent is coke powder; the additive is borax; the water is distilled water, deionized water or ultrapure water.
Comparative example 1
According to the examples in patent application CN 201310123248.2.
Comparative example 2
According to the examples in patent application CN 201310332335.9.
The iron-containing phases prepared in examples 1 to 5 and comparative examples 1 to 2 of the present application were subjected to chemical composition and content analysis, and the contents of the total iron, phosphorus and iron in the iron-containing phase obtained by treating the middle-low grade phosphate ores and copper slags by different methods were recorded, and the experimental results are shown in table 3 below.
TABLE 3
As can be seen from the experimental data in Table 3, the method of the present application can produce ferrophosphorus and gold in accordance with the production requirements.
In conclusion, the invention takes the copper slag resources and the middle-low grade phosphate ores which are not processed and accumulated in large quantity at present as raw materials to prepare the ferrophosphorus alloy material with high added value, and provides a new thought and a new method for the comprehensive utilization of the complex and difficultly processed copper slag and ore resources. The impurity content of the ferrophosphorus alloy is reduced in the treatment process, and the reduction of phosphorus in phosphorite and iron in copper slag is promoted by adding the additive, so that the phosphorus and iron are combined more effectively to form ferrophosphorus material; meanwhile, the reduction temperature can be reduced, the cost is reduced, the energy consumption can be reduced, and the discharge amount of three wastes can be reduced; in addition, the additive has wide sources and low cost, is easy to realize industrial large-scale production, and is particularly suitable for the application of undeveloped medium-low grade phosphorite and copper slag resources. The method provided by the invention comprehensively recycles the medium-low grade phosphorite and the copper slag, changes waste into valuable, improves the resource utilization rate, solves the problems provided by the application, and effectively solves the problems of higher cost, heavy pollution, high energy consumption and large three-waste output when the medium-low grade phosphorite and the copper slag are treated in the prior art. The method has the advantages of low energy consumption, short process flow, high added value of products and wide application prospect, and can better realize the comprehensive utilization of medium and low grade phosphorite and copper slag.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Claims (9)
1. A method for preparing a ferrophosphorus alloy by adopting middle-low grade phosphorite and copper slag is characterized by comprising the following steps: firstly, respectively ball-milling middle-low grade phosphorite and copper slag by adopting a ball mill, then uniformly mixing the medium-low grade phosphorite and copper slag with a reducing agent, an additive and water, firstly sending the mixture into a mould for compression molding under the argon atmosphere, then sending the mixture into a drying box for drying treatment until the water content is 0, and finally sending the mixture into a resistance furnace for roasting, and removing residues by melting to obtain a ferro-phosphorus alloy;
the medium and low grade phosphorite, the copper slag, the reducing agent, the additive and the water are mixed according to the following weight part ratio: 25-35 parts of phosphorite, 60-80 parts of copper slag, 15-17 parts of reducing agent, 4-7 parts of additive and 0.4-0.7 part of water.
2. The method for preparing the ferrophosphorus alloy by using the medium-low grade phosphate ores and the copper slag according to claim 1, is characterized in that: the ball milling is to grind the materials into powder with the granularity of 80-120 meshes.
3. The method for preparing the ferrophosphorus alloy by using the medium-low grade phosphate ores and the copper slag according to claim 1, is characterized in that: the diameter of the die is 20.01-30 mm.
4. The method for preparing the ferrophosphorus alloy by using the medium-low grade phosphate ores and the copper slag according to claim 1, is characterized in that: the pressure of the compression molding is 12-18 MPa.
5. The method for preparing the ferrophosphorus alloy by using the medium-low grade phosphate ores and the copper slag according to claim 1, is characterized in that: the roasting temperature is 1200-1300 ℃, and the roasting time is 60-90 min.
6. The method for preparing the ferrophosphorus alloy by using the medium-low grade phosphate ores and the copper slag according to claim 1, is characterized in that: the drying temperature is not less than 120 ℃, and the drying time is 2-3 h.
7. The method for preparing the ferrophosphorus alloy by using the medium-low grade phosphate ores and the copper slag according to claim 1, is characterized in that: the reducing agent is coke powder.
8. The method for preparing the ferrophosphorus alloy by using the medium-low grade phosphate ores and the copper slag according to claim 1, is characterized in that: the additive is borax.
9. The method for preparing the ferrophosphorus alloy by using the medium-low grade phosphate ores and the copper slag according to claim 1, is characterized in that: the water is distilled water, deionized water or ultrapure water.
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