CN109957661B - Method for recovering chromium from ferronickel smelting slag and preparing light heat-insulating material by microwave reinforcement - Google Patents

Method for recovering chromium from ferronickel smelting slag and preparing light heat-insulating material by microwave reinforcement Download PDF

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CN109957661B
CN109957661B CN201910354773.2A CN201910354773A CN109957661B CN 109957661 B CN109957661 B CN 109957661B CN 201910354773 A CN201910354773 A CN 201910354773A CN 109957661 B CN109957661 B CN 109957661B
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leaching
microwave
slag
chromium
smelting slag
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CN109957661A (en
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彭志伟
李光辉
张元波
古佛全
姜涛
饶明军
苏子键
杨磊
范晓慧
郭宇峰
杨永斌
李骞
徐斌
杨凌志
易凌云
唐慧敏
王连成
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Central South University
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    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B33/00—Clay-wares
    • C04B33/02—Preparing or treating the raw materials individually or as batches
    • C04B33/13—Compounding ingredients
    • C04B33/1305—Organic additives
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B33/00—Clay-wares
    • C04B33/02—Preparing or treating the raw materials individually or as batches
    • C04B33/13—Compounding ingredients
    • C04B33/132—Waste materials; Refuse; Residues
    • C04B33/138—Waste materials; Refuse; Residues from metallurgical processes, e.g. slag, furnace dust, galvanic waste
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
    • C04B35/632—Organic additives
    • C04B35/634—Polymers
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
    • C04B38/02—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by adding chemical blowing agents
    • 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
    • C22B1/00—Preliminary treatment of ores or scrap
    • C22B1/02—Roasting processes
    • 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
    • C22B34/00—Obtaining refractory metals
    • C22B34/30—Obtaining chromium, molybdenum or tungsten
    • C22B34/32—Obtaining chromium
    • 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
    • C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
    • C22B7/006—Wet processes
    • 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
    • C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
    • C22B7/04—Working-up slag
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/74—Physical characteristics
    • C04B2235/77—Density
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
    • C04B2235/9607—Thermal properties, e.g. thermal expansion coefficient
    • 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
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/20—Recycling
    • 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
    • Y02P40/00—Technologies relating to the processing of minerals
    • Y02P40/60—Production of ceramic materials or ceramic elements, e.g. substitution of clay or shale by alternative raw materials, e.g. ashes

Abstract

The invention discloses a method for recovering chromium from ferronickel smelting slag and preparing a light heat-insulating material by microwave reinforcement. Taking the fine ferronickel smelting slag powder as a raw material, taking sodium nitrite and sodium peroxide as additives, and controlling the mass ratio of the ferronickel smelting slag to the sodium nitrite to the sodium peroxide to be 1: (0.2-0.4): (0.3-1.2), uniformly mixing the fine powder of the ferronickel smelting slag with sodium nitrite and sodium peroxide, roasting by microwave, leaching roasted materials by microwave-assisted water, and filtering to obtain chromium-containing leaching liquor and leaching slag. And (3) uniformly mixing the leaching residue with humic acid and water, pressing, forming, drying and roasting by microwave to obtain the light heat-insulating material. The method can realize the selective recovery of chromium in the ferronickel smelting slag and the efficient value-added utilization of the leached slag, and has the advantages of high production efficiency, environmental protection, high product added value and the like.

Description

Method for recovering chromium from ferronickel smelting slag and preparing light heat-insulating material by microwave reinforcement
Technical Field
The invention belongs to the technical field of metallurgy, and particularly relates to a method for recovering chromium from ferronickel smelting slag and preparing a light heat-insulating material through microwave reinforcement.
Background
China is the largest chromium resource consuming country in the world, the chromium consumption is over one third of the world chromite yield, but the annual output of the chromite in China is less than 1% of the world annual output, the huge demand makes the chromium become one of the metals with the highest external dependence in China, and the contradiction between supply and demand is quite prominent.
On the other hand, along with the rapid development of the process for smelting ferronickel from laterite-nickel ore, the discharge amount of ferronickel smelting slag is increased sharply, and according to incomplete statistics, the annual production amount of the ferronickel smelting slag in China exceeds 3000 million tons, the utilization rate of the ferronickel smelting slag is less than 10 percent, and the accumulated stockpiling amount is far more than 2 hundred million tons. The ferronickel smelting slag contains heavy metal elements such as chromium (3 percent) and the like, has potential toxic action, and cannot be widely used in the building material industry like a blast furnace. If the chromium in the ferronickel smelting slag can be recycled, the method has important significance for reducing the external dependence of chromium resources in China and improving the resource utilization water level of the ferronickel smelting slag, and is expected to realize the mass use of the slag after chromium extraction in the material industry and reduce the stockpiling amount of the ferronickel smelting slag.
The method for recovering valuable metals from ferronickel smelting slag mainly comprises a wet process, wherein the wet process is to dissolve elements such as nickel, cobalt, chromium and the like in the slag in an ion form by adopting an acid leaching or alkali fusion method, and then separate and purify valuable components from the solution. In order to separate and recover nickel and chromium from ferronickel smelting slag, research is carried out on enriching nickel in magnetic substances in advance by a magnetic separation method, leaving most chromium in non-magnetic substances, extracting nickel from the magnetic substances by normal-pressure acid leaching, and reacting chromium oxide in the non-magnetic substances with sodium carbonate in an alkali fusion mode to generate sodium chromate easily soluble in water. The result shows that the nickel is enriched from 0.26% to 2.57% and the chromium is enriched from 4.55% to 4.61% after magnetic separation; leaching the magnetic substance for 2 hours at the temperature of 110 ℃ by using 220g/L sulfuric acid solution as a leaching agent, wherein the leaching rate of nickel reaches 91.5%; the non-magnetic material is roasted by sodium carbonate to extract chromium, and the leaching rate of the chromium is 94.1 percent under the conditions that the mass ratio of the sodium carbonate to the non-magnetic material is 0.65, the roasting temperature is 1000 ℃ and the roasting time is 1 h. The method realizes the separation and recovery of nickel and chromium in the ferronickel smelting slag. However, a large amount of leaching slag is generated, and the potential secondary pollution problem is serious.
In conclusion, chromium contained in the ferronickel smelting slag is an important factor influencing the application of the ferronickel smelting slag in the building material industry, and the problems of high roasting temperature, low utilization efficiency, secondary pollution of chromium and the like exist in the existing chromium recovery from the ferronickel smelting slag, so that the development of a more effective recovery process is urgently needed.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a method for recovering chromium from ferronickel smelting slag and preparing a light heat-insulating material by microwave reinforcement.
In order to achieve the technical purpose, the invention adopts the following technical scheme:
the invention relates to a method for recovering chromium from ferronickel smelting slag and preparing a light heat-insulating material by microwave reinforcement, which comprises the following steps:
step one, recovery of chromium
Mixing the fine ferronickel smelting slag powder with sodium nitrite and sodium peroxide to obtain a uniform mixture, carrying out microwave-assisted roasting on the uniform mixture, carrying out water leaching on the obtained roasted material under the assistance of microwave to obtain chromium-containing leachate and leaching slag, wherein the fine ferronickel smelting slag powder is obtained in the uniform mixture according to the mass ratio: sodium nitrite: sodium peroxide is 1, (0.2-0.4): (0.3 to 1.2); the microwave-assisted roasting temperature is 300-450 ℃, the time is 5-20 min,
step two, preparation of light heat insulation material
Adding humic acid and water into the leaching residue obtained in the first step, uniformly mixing, pressing and forming, drying to obtain a briquette, and performing microwave-assisted sintering at the temperature of 600-900 ℃ to obtain the light heat-insulating material.
The key point of the technical scheme of the invention is that the good wave absorbing property of sodium nitrite and sodium peroxide is utilized to realize the rapid integral heating of the mixture of the sodium nitrite and the sodium peroxide and the ferronickel smelting slag, the mass transfer is strengthened, the reaction process is accelerated, the mass ratio and the roasting condition of the ferronickel smelting slag, the sodium nitrite and the sodium peroxide are synchronously controlled, the characteristic that the sodium nitrite is decomposed into the sodium peroxide at low temperature and generates gas is utilized, the mass transfer process is further strengthened, the chromium oxide in the ferronickel smelting slag is selectively converted into the soluble good sodium meta-chromate at low temperature, the rapid and efficient separation of the sodium meta-chromate and other components is realized by the microwave-assisted leaching, the inventor surprisingly discovers that after the obtained leaching slag is uniformly mixed with water, only humic acid as a binding agent is added, and the mixture is pressed and molded, after drying, the light heat-insulating material can be obtained under the condition of extremely low temperature roasting, and the obtained light heat-insulating material has good heat insulation and high strength. In addition, the sintering is carried out under the assistance of microwaves, so that the apparent porosity of the light heat-insulating material can be further improved, the density of the light heat-insulating material is reduced, and in addition, the heating is more uniform in the roasting process, the material defects are few, and the strength is better.
In the invention, sodium nitrite and sodium peroxide cannot be replaced, for example, if sodium hydroxide is selected to replace sodium nitrite or sodium peroxide, although chromium leaching can be realized by raising the temperature and prolonging the time, on one hand, the temperature needs to be raised, hexavalent chromium is generated, the leaching rate is lower, and the prepared material has low porosity and lower strength.
In the invention, the frequency of the microwave is just 2450MHz which is commonly used in the prior art.
In the invention, the fine ferronickel smelting slag powder is obtained by finely grinding ferronickel slag, and the particle size of the fine ferronickel smelting slag powder is less than 74 mu m. Namely, the ferronickel slag is finely ground and then is sieved by a 200-mesh sieve, and the sieved substances are taken out.
In the preferred scheme, in the first step, in the uniform mixture, the fine powder of the ferronickel smelting slag is calculated according to the mass ratio: sodium nitrite: sodium peroxide 1: 0.2-0.3: 0.4 to 0.7.
The inventor finds that the addition amount of sodium nitrite and sodium peroxide has a large influence on chromium recovery rate and subsequent light heat insulation materials, the chromium leaching rate can be slightly increased within a certain range with excessive alkali amount, but effective pore forming cannot be performed, so that the light heat insulation materials are obtained.
In the preferable scheme, in the first step, the microwave roasting temperature is 300-400 ℃ and the time is 5-15 min.
In a preferred scheme, in the step one, the roasted material is ground and then is leached by water, and the ground material is ground to 58-74 μm.
In the invention, the roasting material needs to be further ground, because a small amount of the material is sintered together in the roasting process, the grinding can improve the leaching efficiency and realize quick leaching, but the particle size of the roasting material needs to be effectively controlled, and the roasting material cannot be ground to be too fine (namely, the particle size is too small), otherwise the roasting material is easy to agglomerate, and the leaching efficiency is influenced.
In the preferable scheme, in the first step, the leaching temperature is 25-80 ℃, and the leaching time is 5-30 min.
Preferably, in the step one, the leaching temperature is 40-60 ℃, and the leaching time is 10-20 min.
In the preferred scheme, in the first step, the liquid-solid volume mass ratio of water to the roasted material is 2-8 mL: 1g of the total weight of the composition.
Preferably, in the second step, the addition amount of the humic acid is 2-10 wt% of the mass of the leaching residue.
Preferably, in the second step, the addition amount of the humic acid is 2-5 wt% of the mass of the leaching residue.
Preferably, in the second step, the addition amount of the water is 2-5 wt% of the mass of the leaching residue.
Preferably, in the second step, the pressure of the compression molding is 10-20 MPa.
In the preferable scheme, in the second step, the sintering temperature is 700-800 ℃.
In a preferred scheme, in the second step, the sintering time is 10-50 min.
Preferably, in the second step, the sintering time is 20-30 min.
In the preferred scheme, in the second step, during sintering, the heating rate is 10-25 ℃/min, and the cooling rate is 1-5 ℃/min.
Preferably, in the second step, the temperature rise rate is 15-20 ℃/min and the temperature drop rate is 2-5 ℃/min during sintering.
In the invention, the temperature rising and falling rate of sintering has certain influence on the material performance, and the effectiveness of liquid phase sintering and the formation of pores are influenced by too fast and too slow temperature rising. And the crystallization process can be influenced by too fast temperature reduction, so that the strength of the material is reduced.
The principle and the advantages of the technical scheme of the invention are as follows:
according to the invention, sodium nitrite and sodium peroxide are used as roasting additives of the ferronickel smelting slag for the first time, the recovery of chromium in the ferronickel smelting slag is enhanced by microwaves, and the selective conversion of chromium oxide into sodium meta-chromate with good water solubility is realized by cooperatively controlling the addition amounts of the sodium nitrite and the sodium peroxide and the roasting temperature, so that the efficient selective recovery of chromium is realized. The inventor discovers through a large number of experiments that the mass ratio of the ferronickel smelting slag to the sodium nitrite to the sodium peroxide is controlled to be 1 (0.2-0.4): (0.3-1.2), after being uniformly mixed with sodium nitrite and sodium peroxide, the ferronickel smelting slag fine powder is placed at the temperature of 300-450 ℃ for microwave roasting for 5-20 min, and both the sodium nitrite and the sodium peroxide have excellent wave-absorbing characteristics, so that the whole rapid heating of the mixed and uniform material can be realized under the microwave, the intermolecular motion is accelerated, the sodium nitrite, the sodium peroxide and the ferronickel smelting slag can be rapidly reacted at a reduced temperature, in addition, the mass transfer process is remarkably improved by the liquid phase generated by the sodium nitrite at a low temperature, and the chromium oxide and the sodium peroxide in the ferronickel smelting slag can be rapidly generated into sodium metathromate (NaCrO) which is easy to dissolve in water2) And other components in the slag are insoluble in water, so that the efficient selective recovery of chromium can be realized by microwave-assisted leaching on the premise of not generating hexavalent chromium. Meanwhile, humic acid and water are only added into the leaching residues, and the light heat-insulating material with high strength and low heat conductivity coefficient can be obtained under the condition of extremely low temperature. The method is mainly characterized in that in the chromium removal process, the activity of fine powder of the ferronickel smelting slag is excited by alkali, polymerized aluminosilicate is generated in the microwave roasting process, after humic acid is added into leaching slag, the leaching slag and the humic acid can better play a synergistic effect, the bonding performance is better, the pressed agglomerate is ensured to have good bonding performance and strength before sintering, the humic acid is uniformly and quickly heated and volatilized integrally in the microwave roasting process, a large number of uniformly distributed air holes are formed in the microwave roasting process, the polymerized aluminosilicate in the leaching slag becomes a framework in the cooling process, and high strength is ensured to be obtained, so that the light heat-insulating material with excellent performance is obtained. In addition, the sintering temperature is greatly reduced due to the formation of a liquid phase.
The preparation method disclosed by the invention has the advantages of simple process, high production efficiency, environmental friendliness, high product added value and the like, realizes full-scale efficient utilization of the ferronickel smelting slag, has great economic value and environmental benefit, and has a good application prospect.
Detailed Description
The present invention will be described in detail with reference to the following embodiments, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments, and all other embodiments obtained by those skilled in the art without any inventive work based on the embodiments of the present invention are within the scope of the present invention.
In order to avoid repetition, the raw materials related to this specific embodiment are described below in a unified manner, and are not described in detail in the specific embodiment:
the ferronickel smelting slag comprises the following components in percentage by mass:
SiO228.02-45.15 wt%, 25.41-30.33 wt% of MgO, 5.09-10.26 wt% of FeO, and Al2O33.26-4.53 wt% of Cr2O31.18 to 3.22 wt% and 2.40 to 5.36 wt% of CaO.
The purities of the sodium nitrite and the sodium peroxide are more than 95%.
In the present invention, the frequency of the microwave used is 2450 MHz.
Example 1
And uniformly mixing the fine powder of the ferronickel smelting slag with sodium nitrite and sodium peroxide to obtain a mixture, roasting in a microwave oven, grinding a roasted sample, leaching in a microwave reaction kettle with water, and filtering to obtain leaching slag of the chromium-containing leaching solution. And (3) uniformly mixing the leaching residue with humic acid and water, pressing, forming, drying, firing in a microwave oven, and controlling the temperature rise and fall rate to prepare the light heat-insulating material.
The mass ratio of the fine ferronickel smelting slag powder to the sodium nitrite to the sodium peroxide in the uniform mixture is 1: 0.2: 0.6.
the roasting temperature is 350 ℃.
The roasting time is 15 min.
The leaching temperature was 50 ℃.
The leaching time is 15 min.
The solid-to-liquid ratio of the leaching solution is 8 mL/g.
The calcined sample was ground to an average particle size of 66 μm.
The dosage of the humic acid is 5wt.%, and the dosage of the water is 3 wt.%.
The molding pressure is 10 MPa.
The firing temperature is 800 ℃.
The firing time was 25 min.
The heating rate in the firing process is 15 ℃/min, and the cooling rate is 2 ℃/min.
The chromium leaching rate in example 1 was 98.89%. The obtained light heat insulating material has a refractoriness of 1360 deg.C and a bulk density of 0.79g/cm3The apparent porosity is 63.17%, the thermal conductivity is 0.1011W/(m.K), and the compressive strength is 43.66 MPa.
Example 2
And uniformly mixing the fine powder of the ferronickel smelting slag with sodium nitrite and sodium peroxide to obtain a mixture, roasting in a microwave oven, grinding a roasted sample, leaching in a microwave reaction kettle with water, and filtering to obtain leaching slag of the chromium-containing leaching solution. And (3) uniformly mixing the leaching residue with humic acid and water, pressing, forming, drying, firing in a microwave oven, and controlling the temperature rise and fall rate to prepare the light heat-insulating material.
The mass ratio of the fine ferronickel smelting slag powder to the sodium nitrite to the sodium peroxide in the uniform mixture is 1: 0.2: 0.3.
the roasting temperature is 450 ℃.
The roasting time is 20 min.
The leaching temperature was 80 ℃.
The leaching time is 30 min.
The solid-to-liquid ratio of the leaching solution is 8 mL/g.
The calcined sample was ground to an average particle size of 66 μm.
The dosage of the humic acid is 3 wt.%, and the dosage of the water is 2 wt.%.
The molding pressure is 20 MPa.
The firing temperature is 600 ℃.
The sintering time is 50 min.
In the firing process, the heating rate is 25 ℃/min, and the cooling rate is 5 ℃/min.
In example 2, the chromium leaching rate was 95.36%. The obtained light heat insulating material has refractoriness of 1350 deg.C and volume density of 0.86g/cm3The apparent porosity is 46.61%, the thermal conductivity is 0.1141W/(m.K), and the compressive strength is 34.43 MPa.
Example 3
And uniformly mixing the fine powder of the ferronickel smelting slag with sodium nitrite and sodium peroxide to obtain a mixture, roasting in a microwave oven, grinding a roasted sample, leaching in a microwave reaction kettle with water, and filtering to obtain leaching slag of the chromium-containing leaching solution. And (3) uniformly mixing the leaching residue with humic acid and water, pressing, forming, drying, firing in a microwave oven, and controlling the temperature rise and fall rate to prepare the light heat-insulating material.
The mass ratio of the fine ferronickel smelting slag powder to the sodium nitrite to the sodium peroxide in the uniform mixture is 1: 0.4: 1.0.
the roasting temperature is 300 ℃.
The roasting time is 5 min.
The leaching temperature was 25 ℃.
The leaching time is 5 min.
The solid-to-liquid ratio of the leaching solution is 2 mL/g.
The calcined sample was ground to an average particle size of 58 μm.
The dosage of the humic acid is 2 wt.%, and the dosage of the water is 2 wt.%.
The molding pressure is 10 MPa.
The firing temperature is 900 ℃.
The sintering time is 10 min.
The heating rate in the firing process is 10 ℃/min, and the cooling rate is 1 ℃/min.
In example 3, the chromium leaching rate was 94.66%. The obtained light heat-insulating material is resistant toThe fire degree is 1330 ℃, and the bulk density is 0.90g/cm3The apparent porosity is 42.84%, the thermal conductivity is 0.1297W/(m.K), and the compressive strength is 42.71 MPa.
Example 4
And uniformly mixing the fine powder of the ferronickel smelting slag with sodium nitrite and sodium peroxide to obtain a mixture, roasting in a microwave oven, grinding a roasted sample, leaching in a microwave reaction kettle with water, and filtering to obtain leaching slag of the chromium-containing leaching solution. And (3) uniformly mixing the leaching residue with humic acid and water, pressing, forming, drying, firing in a microwave oven, and controlling the temperature rise and fall rate to prepare the light heat-insulating material.
The mass ratio of the fine ferronickel smelting slag powder to the sodium nitrite to the sodium peroxide in the uniform mixture is 1: 0.2: 0.7.
the roasting temperature is 350 ℃.
The roasting time is 10 min.
The leaching temperature was 55 ℃.
The leaching time is 20 min.
The solid-to-liquid ratio of the leaching solution is 5 mL/g.
The calcined sample was ground to an average particle size of 74 μm.
The dosage of the humic acid is 2 wt.%, and the dosage of the water is 5 wt.%.
The molding pressure is 10 MPa.
The firing temperature is 700 ℃.
The sintering time is 40 min.
The heating rate in the firing process is 20 ℃/min, and the cooling rate is 3 ℃/min.
In example 4, the chromium leaching rate was 96.17%. The obtained light heat insulating material has refractoriness of 1350 deg.C and volume density of 0.85g/cm3The apparent porosity is 50.84%, the thermal conductivity is 0.1297W/(m.K), and the compressive strength is 51.44 MPa.
Example 5
And uniformly mixing the fine powder of the ferronickel smelting slag with sodium nitrite and sodium peroxide to obtain a mixture, roasting in a microwave oven, grinding a roasted sample, leaching in a microwave reaction kettle with water, and filtering to obtain leaching slag of the chromium-containing leaching solution. And (3) uniformly mixing the leaching residue with humic acid and water, pressing, forming, drying, firing in a microwave oven, and controlling the temperature rise and fall rate to prepare the light heat-insulating material.
The mass ratio of the fine ferronickel smelting slag powder to the sodium nitrite to the sodium peroxide in the uniform mixture is 1: 0.4: 0.4.
the roasting temperature is 400 ℃.
The roasting time is 10 min.
The leaching temperature was 40 ℃.
The leaching time is 10 min.
The solid-to-liquid ratio of the leaching solution is 7 mL/g.
The calcined sample was ground to an average particle size of 66 μm.
The dosage of the humic acid is 10wt.%, and the dosage of the water is 3 wt.%.
The molding pressure is 15 MPa.
The firing temperature is 800 ℃.
The sintering time is 20 min.
In the firing process, the heating rate is 25 ℃/min, and the cooling rate is 2 ℃/min.
In example 5, the chromium leaching rate was 96.03%. The obtained light heat-insulating material has a volume refractoriness of 1340 deg.C and a density of 0.90g/cm3The apparent porosity is 65.55%, the thermal conductivity is 0.1009W/(m.K), and the compressive strength is 25.74 MPa.
Comparative example 1
And uniformly mixing the fine ferronickel smelting slag powder with sodium nitrite and sodium peroxide to obtain a mixture, roasting in a muffle furnace, grinding a roasted sample, and filtering after conventional water leaching to obtain chromium-containing leachate. And (3) uniformly mixing the leaching slag with humic acid and water, pressing, forming, drying, sintering in a muffle furnace, and controlling the temperature rise and fall rate to prepare the light heat insulation material.
The mass ratio of the fine ferronickel smelting slag powder to the sodium nitrite to the sodium peroxide in the uniform mixture is 1: 0.2: 0.6.
the roasting temperature is 350 ℃.
The roasting time is 15 min.
The leaching temperature was 50 ℃.
The leaching time is 15 min.
The solid-to-liquid ratio of the leaching solution is 8 mL/g.
The calcined sample was ground to an average particle size of 66 μm.
The dosage of the humic acid is 5wt.%, and the dosage of the water is 3 wt.%.
The molding pressure is 10 MPa.
The firing temperature is 800 ℃.
The firing time was 25 min.
The heating rate in the firing process is 15 ℃/min, and the cooling rate is 2 ℃/min.
The leaching rate of chromium of comparative example 1 was 68.41%. The obtained light heat insulating material has refractoriness of 1350 deg.C and volume density of 0.89g/cm3The apparent porosity was 34.92%, the thermal conductivity was 0.1391W/(m.K), and the compressive strength was 13.66 MPa.
Comparative example 2
And uniformly mixing the fine powder of the ferronickel smelting slag with sodium nitrite and sodium peroxide to obtain a mixture, roasting in a microwave oven, grinding a roasted sample, leaching in a microwave reaction kettle with water, and filtering to obtain leaching slag of the chromium-containing leaching solution. And (3) uniformly mixing the leaching residue with humic acid and water, pressing, forming, drying, firing in a microwave oven, and controlling the temperature rise and fall rate to prepare the light heat-insulating material.
The mass ratio of the fine ferronickel smelting slag powder to the sodium hydroxide and the sodium peroxide in the mixed material is 1: 0.2: 0.6.
the roasting temperature is 350 ℃.
The roasting time is 15 min.
The leaching temperature was 50 ℃.
The leaching time is 15 min.
The solid-to-liquid ratio of the leaching solution is 8 mL/g.
The calcined sample was ground to an average particle size of 58 μm.
The dosage of the humic acid is 5wt.%, and the dosage of the water is 3 wt.%.
The molding pressure is 10 MPa.
The firing temperature is 800 ℃.
The firing time was 25 min.
The heating rate in the firing process is 15 ℃/min, and the cooling rate is 2 ℃/min.
The leaching rate of chromium of this comparative example 2 was 50.36%. The obtained light heat insulating material has refractoriness of 1200 deg.C and bulk density of 1.89g/cm3The apparent porosity was 14.29%, the thermal conductivity was 0.5304W/(m.K), and the compressive strength was 14.74 MPa.
Comparative example 3
And uniformly mixing the fine powder of the ferronickel smelting slag with sodium nitrite and sodium peroxide to obtain a mixture, roasting in a microwave oven, grinding a roasted sample, leaching in a microwave reaction kettle with water, and filtering to obtain leaching slag of the chromium-containing leaching solution. And (3) uniformly mixing the leaching residue with humic acid and water, pressing, forming, drying, firing in a microwave oven, and controlling the temperature rise and fall rate to prepare the light heat-insulating material.
The mass ratio of the fine ferronickel smelting slag powder to the sodium nitrite to the sodium hydroxide in the uniform mixture is 1: 0.2: 0.6.
the roasting temperature is 350 ℃.
The roasting time is 15 min.
The leaching temperature was 50 ℃.
The leaching time is 15 min.
The solid-to-liquid ratio of the leaching solution is 8 mL/g.
The calcined sample was ground to an average particle size of 58 μm.
The dosage of the humic acid is 5wt.%, and the dosage of the water is 3 wt.%.
The molding pressure is 10 MPa.
The firing temperature is 800 ℃.
The firing time was 25 min.
The heating rate in the firing process is 15 ℃/min, and the cooling rate is 2 ℃/min.
The leaching rate of chromium in comparative example 3 was 52.30%. The obtained light heat-insulating material has refractoriness of 1100 deg.C and bulk density of 2.08g/cm3The apparent porosity was 12.89%, the thermal conductivity was 0.5373W/(m.K), and the compressive strength was 16.78 MPa.
Comparative example 4
And uniformly mixing the fine powder of the ferronickel smelting slag with sodium nitrite and sodium peroxide to obtain a mixture, roasting in a microwave oven, grinding a roasted sample, leaching in a microwave reaction kettle with water, and filtering to obtain leaching slag of the chromium-containing leaching solution. And (3) uniformly mixing the leaching residue with humic acid and water, pressing, forming, drying, firing in a microwave oven, and controlling the temperature rise and fall rate to prepare the light heat-insulating material.
The mass ratio of the fine ferronickel smelting slag powder to the sodium nitrite to the sodium peroxide in the uniform mixture is 1: 0.1: 0.2.
the roasting temperature is 350 ℃.
The roasting time is 15 min.
The leaching temperature was 50 ℃.
The leaching time is 15 min.
The solid-to-liquid ratio of the leaching solution is 8 mL/g.
The calcined sample was ground to an average particle size of 66 μm.
The dosage of the humic acid is 5wt.%, and the dosage of the water is 3 wt.%.
The molding pressure is 10 MPa.
The firing temperature is 800 ℃.
The firing time was 25 min.
The heating rate in the firing process is 15 ℃/min, and the cooling rate is 2 ℃/min.
The leaching rate of chromium of comparative example 4 was 32.07%. The obtained light heat-insulating material has refractoriness of 1100 deg.C and bulk density of 2.48g/cm3The apparent porosity was 11.98%, the thermal conductivity was 0.5437W/(m.K), and the compressive strength was 36.74 MPa.
Comparative example 5
And uniformly mixing the fine powder of the ferronickel smelting slag with sodium nitrite and sodium peroxide to obtain a mixture, roasting in a microwave oven, grinding a roasted sample, leaching in a microwave reaction kettle with water, and filtering to obtain leaching slag of the chromium-containing leaching solution. And (3) uniformly mixing the leaching residue with humic acid and water, pressing, forming, drying, firing in a microwave oven, and controlling the temperature rise and fall rate to prepare the light heat-insulating material.
The mass ratio of the fine ferronickel smelting slag powder to the sodium nitrite to the sodium peroxide in the uniform mixture is 1: 0.5: 1.5.
the roasting temperature is 300 ℃.
The roasting time is 15 min.
The leaching temperature was 50 ℃.
The leaching time is 15 min.
The solid-to-liquid ratio of the leaching solution is 8 mL/g.
The calcined sample was ground to an average particle size of 58 μm.
The dosage of the humic acid is 5wt.%, and the dosage of the water is 3 wt.%.
The molding pressure is 10 MPa.
The firing temperature is 500 ℃.
The sintering time is 15 min. The heating rate in the firing process is 15 ℃/min, and the cooling rate is 2 ℃/min.
The leaching rate of chromium of this comparative example 5 was 95.63%. The obtained light heat-insulating material has refractoriness of 1100 deg.C and volume density of 1.85g/cm3The apparent porosity was 29.28%, the thermal conductivity was 0.3743W/(m.K), and the compressive strength was 29.78 MPa.
Comparative example 6
And uniformly mixing the fine powder of the ferronickel smelting slag with sodium nitrite and sodium peroxide to obtain a mixture, roasting in a microwave oven, grinding a roasted sample, leaching in a microwave reaction kettle with water, and filtering to obtain leaching slag of the chromium-containing leaching solution. And (3) uniformly mixing the leaching residue with humic acid and water, pressing, forming, drying, firing in a microwave oven, and controlling the temperature rise and fall rate to prepare the light heat-insulating material.
The mass ratio of the fine ferronickel smelting slag powder to the sodium nitrite to the sodium peroxide in the uniform mixture is 1: 0.2: 0.6.
the roasting temperature is 350 ℃.
The roasting time is 4 min.
The leaching temperature was 50 ℃.
The leaching time is 4 min.
The solid-to-liquid ratio of the leaching solution is 8 mL/g.
The calcined sample was ground to an average particle size of 66 μm.
The dosage of the humic acid is 5wt.%, and the dosage of the water is 3 wt.%.
The molding pressure is 20 MPa.
The firing temperature is 1000 ℃.
The sintering time is 60 min.
The heating rate in the firing process is 30 ℃/min, and the cooling rate is 2 ℃/min.
The leaching rate of chromium of this comparative example 6 was 60.66%. The obtained light heat insulating material has refractoriness of 1150 deg.C and bulk density of 2.68g/cm3The apparent porosity was 9.89%, the thermal conductivity was 0.5833W/(m.K), and the compressive strength was 58.04 MPa.
Comparative example 7
And uniformly mixing the fine powder of the ferronickel smelting slag with sodium nitrite and sodium peroxide to obtain a mixture, roasting in a microwave oven, grinding a roasted sample, leaching in a microwave reaction kettle with water, and filtering to obtain leaching slag of the chromium-containing leaching solution. And (3) uniformly mixing the leaching residue with humic acid and water, pressing, forming, drying, firing in a microwave oven, and controlling the temperature rise and fall rate to prepare the light heat-insulating material.
The mass ratio of the fine ferronickel smelting slag powder to the sodium nitrite to the sodium peroxide in the uniform mixture is 1: 0.2: 0.6.
the roasting temperature is 250 ℃.
The roasting time is 20 min.
The leaching temperature was 80 ℃.
The leaching time is 30 min.
The solid-to-liquid ratio of the leaching solution is 8 mL/g.
The calcined sample was ground to an average particle size of 66 μm.
The dosage of the humic acid is 5wt.%, and the dosage of the water is 3 wt.%.
The molding pressure is 10 MPa.
The firing temperature is 800 ℃.
The firing time was 25 min.
The heating rate in the firing process is 15 ℃/min, and the cooling rate is 2 ℃/min.
The leaching rate of chromium of this comparative example 7 was 45.78%. The obtained light heat insulating material has refractoriness of 1150 deg.C and bulk density of 1.48g/cm3The apparent porosity was 29.12%, the thermal conductivity was 0.5364W/(m.K), and the compressive strength was 29.74 MPa.
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, and it is therefore intended that the present embodiments 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.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art will be able to make the description as a whole, and the embodiments in each example may be appropriately combined to form other embodiments that may be understood by those skilled in the art.

Claims (8)

1. A method for recovering chromium from ferronickel smelting slag and preparing light heat insulation materials by microwave reinforcement is characterized by comprising the following steps: the method comprises the following steps:
step one, recovery of chromium
Mixing the fine ferronickel smelting slag powder with sodium nitrite and sodium peroxide to obtain a mixed material, carrying out microwave-assisted roasting on the mixed material, carrying out water leaching on the obtained roasted material under the assistance of microwave to obtain chromium-containing leachate and leaching slag, wherein the fine ferronickel smelting slag powder comprises the following components in percentage by mass: sodium nitrite: sodium peroxide =1 (0.2-0.4): (0.3 to 1.2); the microwave isThe temperature of the auxiliary roasting is 300-450 DEGoC, the time is 5-20 min,
step two, preparation of light heat insulation material
Adding humic acid and water into the leaching residue obtained in the first step, uniformly mixing, pressing and forming, drying to obtain a briquette, and performing microwave-assisted sintering to obtain the light heat-insulating material, wherein the addition amount of the humic acid is 2-10 wt% of the mass of the leaching residue, and the temperature of the microwave-assisted sintering is 600-900%oC; during sintering, the heating rate is 10-25oC/min, cooling rate of 1-5oC/min。
2. The method for the microwave enhanced chromium recovery from ferronickel slag and the production of lightweight thermal insulation material according to claim 1, characterized in that: in the first step, in the uniform mixture, the fine powder of the ferronickel smelting slag is calculated according to the mass ratio: sodium nitrite: sodium peroxide =1: 0.2-0.3: 0.4 to 0.7.
3. The method for the microwave enhanced chromium recovery from ferronickel slag and the production of lightweight thermal insulation material according to claim 1, characterized in that: in the first step, the roasted material is ground and then is leached by water, and the ground material is ground to 58-74 mu m.
4. The method for the microwave enhanced chromium recovery from ferronickel slag and the production of lightweight thermal insulation material according to claim 1, characterized in that: in the first step, the leaching temperature is 25-80 DEG CoAnd C, leaching for 5-30 min.
5. The method for the microwave enhanced chromium recovery from ferronickel slag and the production of lightweight thermal insulation material according to claim 1, characterized in that: in the first step, during leaching, the liquid-solid volume mass ratio of water to roasted materials is 2-8 mL: 1g of the total weight of the composition.
6. The method for the microwave enhanced chromium recovery from ferronickel slag and the production of lightweight thermal insulation material according to claim 1, characterized in that: in the second step, the addition amount of the water is 2-5 wt% of the mass of the leaching residue.
7. The method for the microwave enhanced chromium recovery from ferronickel slag and the production of lightweight thermal insulation material according to claim 1, characterized in that: the pressure of the compression molding is 10-20 MPa.
8. The method for the microwave enhanced chromium recovery from ferronickel slag and the production of lightweight thermal insulation material according to claim 1, characterized in that: in the second step, the sintering temperature is 700-800 DEG CoAnd C, sintering for 10-50 min.
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