CN110760681B - Method for extracting sulfuric acid and nickel-chromium-iron alloy from stainless steel pickling waste liquid - Google Patents
Method for extracting sulfuric acid and nickel-chromium-iron alloy from stainless steel pickling waste liquid Download PDFInfo
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- CN110760681B CN110760681B CN201911062940.2A CN201911062940A CN110760681B CN 110760681 B CN110760681 B CN 110760681B CN 201911062940 A CN201911062940 A CN 201911062940A CN 110760681 B CN110760681 B CN 110760681B
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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
- 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
- C22B7/001—Dry processes
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B17/00—Sulfur; Compounds thereof
- C01B17/69—Sulfur trioxide; Sulfuric acid
- C01B17/74—Preparation
- C01B17/76—Preparation by contact processes
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21B—MANUFACTURE OF IRON OR STEEL
- C21B13/00—Making spongy iron or liquid steel, by direct processes
- C21B13/0006—Making spongy iron or liquid steel, by direct processes obtaining iron or steel in a molten state
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21B—MANUFACTURE OF IRON OR STEEL
- C21B13/00—Making spongy iron or liquid steel, by direct processes
- C21B13/0066—Preliminary conditioning of the solid carbonaceous reductant
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21B—MANUFACTURE OF IRON OR STEEL
- C21B13/00—Making spongy iron or liquid steel, by direct processes
- C21B13/08—Making spongy iron or liquid steel, by direct processes in rotary furnaces
- C21B13/085—Making spongy iron or liquid steel, by direct processes in rotary furnaces wherein iron or steel is obtained in a molten state
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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
- C22B1/00—Preliminary treatment of ores or scrap
- C22B1/11—Removing sulfur, phosphorus or arsenic other than by roasting
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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
- C22B23/00—Obtaining nickel or cobalt
- C22B23/02—Obtaining nickel or cobalt by dry processes
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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
- C22B34/00—Obtaining refractory metals
- C22B34/30—Obtaining chromium, molybdenum or tungsten
- C22B34/32—Obtaining chromium
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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
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
- C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
- C23G1/36—Regeneration of waste pickling liquors
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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
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention relates to a method for extracting sulfuric acid and nickel-chromium-iron alloy from stainless steel pickling waste liquid, wherein the stainless steel pickling waste liquid is prepared by adding carbon powder into sulfate crystals separated by a freezing-acid regulating crystallization method, then feeding the sulfate crystals into a rotary heating furnace for heating, so that the sulfate crystals separate out crystal water and carry out decomposition reaction to generate solid products such as ferric oxide, nickel oxide, chromium oxide and the like and gas products such as sulfur dioxide, sulfur trioxide, oxygen and the like, feeding the solid products and the carbon powder into an induction heating furnace for high-temperature heating, carrying out melting reduction and alloying to form the nickel-chromium-iron alloy, feeding the gas products into a tail gas purifying furnace, oxidizing the sulfur dioxide into gas under the action of high temperature and catalyst, reacting with the sulfur trioxide in a quenching heat exchange device to generate sulfuric acid, and the extracted sulfuric acid and nickel-chromium-iron alloy can be reused as pickling and smelting raw, realizes the reutilization of waste, reduces the production cost and the environmental pollution, and has remarkable economic benefit.
Description
Technical Field
The invention relates to the technical field of stainless steel pickling waste liquid treatment, in particular to a method for extracting sulfuric acid and nickel-chromium-iron alloy from stainless steel pickling waste liquid.
Background
In the production of stainless steel, 10-20% sulfuric acid is usually used to remove oxide skin and rust on the surface of stainless steel, and the pickling waste liquid contains sulfuric acid and sulfates of metallic iron, nickel, chromium, etc., and is discharged after being treated as sewage in the early stage, thereby causing great waste and environmental pollution. At present, various iron and steel enterprises take stainless steel pickling waste liquid as renewable resources for realizing resource recycling and actively develop the technology for treating the stainless steel pickling waste liquid.
There are many treatment techniques for waste liquid produced by pickling stainless steel with sulfuric acid, for example: concentration-filtrationThe method comprises a natural crystallization method, an immersion combustion high-temperature crystallization method, a steam jet vacuum crystallization method, an evaporation concentration-cooling crystallization method, an acid adjusting-freezing crystallization method, an alkali liquor-ferrous sulfate coprecipitation method and the like, wherein the acid adjusting-freezing crystallization method has the advantages of shorter process flow, less equipment investment, less energy consumption, lower running cost, simple operation, no secondary pollution and the like, and is applied to a plurality of steel plants. The method comprises precipitating most of metal ions in the form of sulfate crystal (FeS 0) containing ferrous sulfate as main component4·7H20) The content is about 61.2%, the content of nickel sulfate crystals is about 4.99%, and the content of chromium sulfate crystals is about 9.48%. The sulfates are commonly used as wastes in steel mills, and cause environmental pollution if being landfilled, so that the sulfates are not allowed by the current environmental protection; if the price is low when the reagent is sold as a chemical reagent, the economic benefit is not high.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a method for extracting sulfuric acid and nickel-chromium-iron alloy from stainless steel pickling waste liquid, which can convert noble metal ions such as nickel, chromium and the like in sulfate crystals into nickel-chromium-iron alloy and sulfate radicals into sulfuric acid, thereby realizing the recycling of wastes, reducing the production cost, reducing the environmental pollution and having obvious economic benefit.
In order to achieve the purpose, the invention adopts the technical scheme that: a method for extracting sulfuric acid and nickel-chromium-iron alloy from stainless steel pickling waste liquid comprises the following steps:
firstly, separating sulfate crystals of metal iron, nickel and chromium from the stainless steel pickling waste liquid by adopting a freezing-acid regulating crystallization method;
secondly, crushing the sulfate crystals obtained in the first step, adding carbon powder in a proper proportion, feeding the crushed sulfate crystals into a rotary heating furnace, heating the crushed sulfate crystals, separating out crystal water from the sulfate crystals in a low-temperature region, and carrying out decomposition reaction on the sulfate in a high-temperature region to generate solid products including iron oxide, nickel oxide and chromium oxide and gas products including sulfur dioxide, sulfur trioxide and oxygen;
step three, feeding the solid product and the carbon powder generated in the rotary heating furnace in the step two into an induction heating furnace for high-temperature heating, reducing the metal oxide into liquid metal of iron, nickel and chromium by the carbon powder at high temperature, and simultaneously completing desulfurization, deoxidation and decarburization; then alloying and smelting the liquid metal of iron, nickel and chromium at high temperature to form nickel-chromium-iron alloy;
and step four, the gas product generated in the rotary heating furnace in the step two is sent into a tail gas purifying furnace, under the action of high temperature and catalyst, sulfur dioxide is absorbed into oxygen in the tail gas purifying furnace and is oxidized into sulfur trioxide gas, a water spray cooling mode is adopted in a quenching heat exchange device, and concentrated sulfuric acid is adopted as an absorbent at the same time, so that the sulfur trioxide gas reacts with water to generate sulfuric acid.
Further, the sulfate crystals in the first step comprise ferrous sulfate crystals FeSO4·7H2O, nickel sulfate crystal NiSO4·6H2O and chromium sulfate crystal Cr2(SO4)35, 12, 18 hydrate of (1).
Further, the proportion of the carbon powder added in the second step is 5 percent.
Further, the rotary heating furnace in the step two adopts a rotary electric furnace, so that the material can move forwards while being heated, and the heating temperature in the furnace is controlled to be 500-.
Further, nitrogen is introduced into an air inlet of the rotary heating furnace in the step two, air exhaust is carried out by a high-temperature centrifugal machine at an air outlet, and gas products generated by heating reaction in the rotary heating furnace can be rapidly discharged: the water vapor, the sulfur dioxide, the sulfur trioxide and the oxygen enable the reaction to be rapid and complete, and simultaneously prevent external oxygen from entering to influence the chemical reaction and prevent carbon powder from being oxidized.
Further, the induction heating furnace in the third step adopts nitrogen as protective atmosphere, and the temperature in the furnace is controlled at 1450-1600 ℃.
Further, the temperature in the tail gas purifying furnace in the fourth step is controlled at 750-900 ℃, and the catalyst is vanadium pentoxide V2O5。
Furthermore, in the fourth step, 98.3% concentrated sulfuric acid is used as an absorbent.
Has the advantages that: the method provided by the invention can be used for treatment and recycling production of the stainless steel pickling waste liquid, can extract sulfuric acid and the nickel-chromium-iron alloy from sulfate crystals precipitated from the stainless steel pickling waste liquid, can reuse the sulfuric acid for pickling production of the stainless steel, can reuse the nickel-chromium-iron alloy as a raw material for producing the stainless steel, effectively realizes waste recycling, and has the advantages of environmental protection, high economic benefit and the like compared with the prior art.
Drawings
FIG. 1 is a schematic diagram of the extraction process of the present invention;
fig. 2 is a schematic diagram of the working principle of the embodiment of the invention.
Detailed Description
The invention is described in further detail below with reference to the figures and specific examples.
The technical principle of the method for extracting sulfuric acid and nickel-chromium-iron alloy from stainless steel pickling waste liquid is shown in figure 1, the stainless steel pickling waste liquid is subjected to freezing-acid adjusting crystallization to separate sulfate crystals of metallic iron, nickel and chromium, mainly ferrous sulfate crystals (FeSO)4·7H2O), nickel sulfate crystal (NiSO)4·6H2O), chromium sulfate crystal (Cr)2(SO4)3Hydrate 5, 12, 18) of the above-mentioned sulfate salt, the sulfate salt crystals are pulverized and then carbon powder is added in an appropriate ratio and fed into a heating furnace to be heated, so that the sulfate salt crystals are precipitated as crystal water, and then decomposition reaction is carried out to produce iron oxide (Fe)2O3) Nickel oxide (NiO), chromium oxide (Cr)2O3) Equal solid product and sulfur dioxide (SO)2) Sulfur trioxide (SO)3) Oxygen (O)2) And (3) the gaseous product, the chemical reaction equation of which is shown in the following formulas (1) to (6):
metal oxide (Fe) generated in a heating furnace2O3、NiO、Cr2O3) Feeding solid such as carbon powder and the like into an induction heating furnace for high-temperature heating; firstly, melting and reducing the raw materials, reducing the metal oxides into liquid metals of iron, nickel and chromium by carbon powder at high temperature, and simultaneously completing desulfurization, deoxidation, decarburization and the like, wherein reaction equations are shown in formulas (7) to (9); then alloying the metals at high temperature, and alloying and smelting the liquid metals of iron, nickel and chromium to form the nickel-chromium-iron alloy which can be used as a raw material to be reused in the smelting production of stainless steel.
The gas product generated in the heating furnace is sent into a tail gas purifying furnace, under the action of high temperature and a catalyst, sulfur dioxide is absorbed into oxygen in the tail gas purifying furnace and is oxidized into sulfur trioxide gas, and the reaction equation is shown as the formula (10); a water spray cooling mode is adopted in the quenching heat exchange device, sulfur trioxide gas reacts with water to generate sulfuric acid, a reaction equation is shown as a formula (11), the concentration of the sulfuric acid is determined by the water quantity, and the generated sulfuric acid can be reused for stainless steel pickling.
H2O+SO3＝＝H2SO4 (11)
Example 1
The working principle diagram of the specific embodiment of the invention is shown in fig. 2, and the equipment adopted in the embodiment for extracting sulfuric acid and nickel-chromium-iron alloy mainly comprises a high-temperature screw feeder, a rotary heating furnace, an induction heating furnace, a cooling device, a high-temperature centrifugal fan, a tail gas purification furnace, a quenching heat exchange device and the like.
The stainless steel pickling waste liquid is frozen and acid regulated to crystallize to separate out sulfate crystal of Fe, Ni and Cr, which is crushed and added with about 5% carbon powder, mixed and fed into rotary heating furnace for heating.
The rotary heating furnace adopts a rotary electric furnace, so that the material can move forwards while being heated, the heating temperature in the furnace is controlled at 900 ℃, the crystal water can be separated out from the sulfate crystal in a low temperature region, and the sulfate can generate decomposition reaction in a high temperature region to generate iron oxide (Fe)2O3) Nickel oxide (NiO), chromium oxide (Cr)2O3) Equal solid and sulfur dioxide (SO)2) Sulfur trioxide (SO)3) Oxygen (O)2) And the chemical reaction equations of the gases are shown in the above formulas (1) to (6). Introducing nitrogen (N) into the air inlet of the rotary heating furnace2) The exhaust port is used for exhausting air by a high-temperature centrifugal machine, and the air can be quickly discharged out of the heating furnace for heating reactionThe steam, sulfur dioxide, sulfur trioxide, oxygen and other gases of output make the reaction go on rapidly and completely, prevent simultaneously that outside oxygen from getting into and influencing the chemical reaction, prevent that the carbon dust from being oxidized.
Metal oxide (Fe) produced in rotary furnace2O3、NiO、Cr2O3) And solid such as carbon powder and the like are fed into the induction heating furnace from the discharge port to be heated at high temperature. The induction heating furnace adopts nitrogen (N)2) As a protective atmosphere, the temperature in the furnace is controlled at 1450-1600 ℃, the raw materials can be melted and reduced, the metal oxide is reduced by carbon powder at high temperature to form liquid metal of iron, nickel and chromium, the reaction equation is shown in the formulas (7) to (9), and the desulfurization, the deoxidation, the decarburization and the like are simultaneously completed; then alloying the metals at high temperature, and alloying and smelting the liquid metals of iron, nickel and chromium to form nickel-chromium-iron alloy; the liquid alloy is solidified into solid nickel-chromium-iron alloy after passing through the cooling device, and the nickel-chromium-iron alloy can be used as a raw material to be reused in the smelting production of stainless steel.
The gas product generated in the rotary heating furnace is sent into the tail gas purifying furnace from the exhaust port of the rotary heating furnace under the action of the high-temperature centrifuge, and meanwhile, the external air is also sucked into the tail gas purifying furnace. The temperature of the tail gas purification furnace is controlled at 750-2O5) As a catalyst, sulfur dioxide is oxidized by oxygen in the furnace to sulfur trioxide gas at elevated temperatures, the reaction equation being shown above in equation (10).
The method comprises the following steps that sulfur trioxide gas generated in a tail gas purification furnace enters rapid cooling heat exchange equipment, external cooling water enters the rapid cooling heat exchange equipment, the sulfur trioxide gas in the rapid cooling heat exchange equipment is cooled in a water spray cooling mode, 98.3% concentrated sulfuric acid is used as an absorbent, the sulfur trioxide gas can react with water to generate sulfuric acid, a reaction equation is shown as a formula (11), and the concentration of the generated sulfuric acid is determined by the amount of cooling water; the cooling water amount is usually adjusted to generate dilute sulfuric acid with the concentration of 10-20 percent, and the dilute sulfuric acid is reused for the pickling production of stainless steel.
The invention converts sulfate crystals precipitated from the pickling waste liquid in the stainless steel production into sulfuric acid and nickel-chromium-iron alloy, and the sulfate crystals can be reused in the stainless steel production as pickling and smelting raw materials, thereby realizing the reutilization of wastes, reducing the production cost and the environmental pollution and having remarkable economic benefit.
Although the present invention has been described with reference to a preferred embodiment, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (8)
1. A method for extracting sulfuric acid and nickel-chromium-iron alloy from stainless steel pickling waste liquid is characterized by comprising the following steps: the method comprises the following steps:
firstly, separating sulfate crystals of metal iron, nickel and chromium from the stainless steel pickling waste liquid by adopting a freezing-acid regulating crystallization method;
secondly, crushing the sulfate crystals obtained in the first step, adding carbon powder in a proper proportion, feeding the crushed sulfate crystals into a rotary heating furnace, heating the rotary heating furnace at the temperature of 500-900 ℃, separating out crystal water from the sulfate crystals in a low-temperature zone, and carrying out decomposition reaction on the sulfate in a high-temperature zone to generate solid products including iron oxide, nickel oxide and chromium oxide and gas products including sulfur dioxide, sulfur trioxide and oxygen;
step three, the solid product and the carbon powder generated in the rotary heating furnace in the step two are sent into an induction heating furnace for high-temperature heating, the temperature in the induction heating furnace is controlled at 1450-1600 ℃, the metal oxide is reduced into liquid metal of iron, nickel and chromium by the carbon powder at high temperature, and simultaneously, the desulfurization, the deoxidation and the decarburization are completed; then alloying and smelting the liquid metal of iron, nickel and chromium at high temperature to form nickel-chromium-iron alloy;
and step four, the gas product generated in the rotary heating furnace in the step two is sent into a tail gas purifying furnace, the temperature in the tail gas purifying furnace is controlled at 750-plus-900 ℃, under the action of high temperature and catalyst, sulfur dioxide is absorbed into oxygen in the tail gas purifying furnace and is oxidized into sulfur trioxide gas, a water spray cooling mode is adopted in a quenching heat exchange device, and meanwhile, concentrated sulfuric acid is adopted as an absorbent to enable the sulfur trioxide gas to react with water to generate sulfuric acid.
2. The method of claim 1, wherein the sulfate crystals in step one comprise FeSO crystals4·7H2O, nickel sulfate crystal NiSO4·6H2O and chromium sulfate crystal Cr2(SO4)35, 12, 18 hydrate of (1).
3. The method for extracting sulfuric acid and nickel-chromium-iron alloy from stainless steel pickling waste liquid according to claim 1, wherein the proportion of the carbon powder added in the second step is 5%.
4. The method for extracting sulfuric acid and nickel-chromium-iron alloy from stainless steel pickling waste liquid according to claim 1, wherein the rotary heating furnace in the second step is a rotary electric furnace, and the material can move forward while being heated.
5. The method for extracting sulfuric acid and nickel-chromium-iron alloy from stainless steel pickling waste liquor as claimed in claim 1, wherein in the second step, nitrogen is introduced into the air inlet of the rotary heating furnace, and the air exhaust is performed by a high-temperature centrifuge, so that gas products generated by the heating reaction in the rotary heating furnace can be rapidly exhausted: the water vapor, the sulfur dioxide, the sulfur trioxide and the oxygen enable the reaction to be rapid and complete, and simultaneously prevent external oxygen from entering to influence the chemical reaction and prevent carbon powder from being oxidized.
6. The method for extracting sulfuric acid and nickel-chromium-iron alloy from stainless steel pickling waste liquid according to claim 1, wherein the induction heating furnace in the third step adopts nitrogen as protective atmosphere.
7. The method for extracting sulfuric acid and nickel-chromium-iron alloy from stainless steel pickling waste liquid according to claim 1, wherein the catalyst in the fourth step is vanadium pentoxide V2O5。
8. The method for extracting sulfuric acid and nickel-chromium-iron alloy from stainless steel pickling waste liquid according to claim 1, wherein in the fourth step, 98.3% concentrated sulfuric acid is used as an absorbent.
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| CN113511634B (en) * | 2021-05-08 | 2023-11-10 | 佛山市景嘉机电设备有限公司 | System and method for preparing sulfuric acid by recycling waste ferric sulfate crude salt in steel industry through pickling |
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| CN103058150B (en) * | 2012-12-12 | 2015-03-11 | 刘立文 | Producing method of sulfuric acid by using calcium sulfate under high temperature and high pressure |
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