CN110734238A - method for synergistically recovering red mud and desulfurized fly ash, filler, cementing material and preparation method - Google Patents
method for synergistically recovering red mud and desulfurized fly ash, filler, cementing material and preparation method Download PDFInfo
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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
- C04B20/00—Use of materials as fillers for mortars, concrete or artificial stone according to more than one of groups C04B14/00 - C04B18/00 and characterised by shape or grain distribution; Treatment of materials according to more than one of the groups C04B14/00 - C04B18/00 specially adapted to enhance their filling properties in mortars, concrete or artificial stone; Expanding or defibrillating materials
- C04B20/02—Treatment
- C04B20/04—Heat treatment
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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
- C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
- C04B28/14—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing calcium sulfate cements
- C04B28/142—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing calcium sulfate cements containing synthetic or waste calcium sulfate cements
- C04B28/144—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing calcium sulfate cements containing synthetic or waste calcium sulfate cements the synthetic calcium sulfate being a flue gas desulfurization product
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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
- C04B40/00—Processes, in general, for influencing or modifying the properties of mortars, concrete or artificial stone compositions, e.g. their setting or hardening ability
- C04B40/0028—Aspects relating to the mixing step of the mortar preparation
- C04B40/0039—Premixtures of ingredients
- C04B40/0046—Premixtures of ingredients characterised by their processing, e.g. sequence of mixing the ingredients when preparing the premixtures
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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
- C22B1/02—Roasting processes
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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
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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
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/91—Use of waste materials as fillers for mortars or concrete
Abstract
The invention discloses a method for cooperatively recovering red mud and desulfurization ash, a filler, a cementing material and a preparation method, and relates to the technical field of resource utilization of industrial waste residues.
Description
Technical Field
The invention relates to the technical field of resource utilization of industrial waste residues, in particular to a method for recycling types of red mud and desulfurized fly ash in a synergistic manner, a filler, a cementing material and a preparation method.
Background
According to the statistics of the international alumina society, the alumina yield in China is increased in a well-jet mode in nearly 10 years, the annual alumina yield is increased from 851 ten thousand tons in 2005 to 5897 ten thousand tons in 2015, along with the generation of a large amount of red mud, according to incomplete estimation, 1-2t of red mud is generated per 1t of alumina produced on average, in recent years, the annual emission amount of the Chinese red mud exceeds 5000 ten thousand tons, the cumulative inventory amount of the red mud exceeds 3 hundred million tons, the red mud is also classified as large industrial solid waste, about 27 million tons of red mud are generated in the global history of producing alumina by an alkaline process for more than 120 years, and the quantity of the red mud is increased by 1.2 million tons per year, and the treatment and resource utilization of the red mud are huge problems faced by the alumina industry.
The semi-dry sintering flue gas desulfurization ash is kinds of solid wastes finally generated by using the semi-dry sintering flue gas desulfurization technology, is mainly a desulfurization byproduct separated from dust removal equipment after the reaction of sulfur-containing components in the sintering flue gas and a calcium-based desulfurizing agent, and contains a large amount of CaSO3CaSO in the dried state3Stable physical and chemical properties and difficult oxidation or decomposition reaction. However, CaSO in a moist state3Very poor in physical and chemical propertiesIs stable, is very easy to be oxidized in the air, and generates calcium sulfate (CaSO) with stable property, compact structure4) An oxidation product layer as a main component. Therefore, when the sintered flue gas desulfurization ash is used as a raw material for preparing building materials such as cement concrete and the like, CaSO is generated3The hydration reaction is carried out to generate crystal water, so that the building material is slightly expanded, and the security of the building material is threatened.
In view of this, the invention is particularly proposed.
Disclosure of Invention
The invention aims to provide methods for synergistically recovering red mud and desulfurized fly ash, a filler, a cementing material and a preparation method so as to solve the technical problems.
The invention is realized by the following steps:
method for synergistically recovering red mud and desulfurized fly ash, which comprises the following steps of mixing red mud and desulfurized fly ash and then calcining.
The method is characterized in that the red mud which is an intermediate product in the alumina production process and the desulfurized fly ash which is a solid waste are calcined, iron oxide in the red mud has the characteristic of catalytic oxidation, the iron oxide can oxidize calcium sulfite in the desulfurized fly ash into calcium sulfate, and the iron oxide is reduced into magnetite (mainly Fe)3O4). The produced magnetite can be used for steel smelting and other purposes. The method can greatly consume the red mud, not only realizes cost reduction and efficiency improvement of steel, but also solves the problems of red mud emission and treatment, and improves economic benefits and environmental benefits.
In the embodiment with the better application of the invention, the mass ratio of the red mud to the desulfurized fly ash in the method is 2-6: 1;
preferably, the mass ratio of the red mud to the desulfurized fly ash in the method is 3: 1.
The mass ratio of the red mud to the desulfurized fly ash is determined by an oxidation-reduction reaction equation, and within the range of the addition mass ratio, the hematite (iron oxide) in the red mud can be fully reduced into magnetite (Fe)3O4) And the recovery rate of magnetite from red mud is improved.
CaO and Ca (OH) in desulfurized fly ash2Sum of mass percent20 to 40 percent of CaSO3The mass percentage content is 30-60%, the granularity is less than 45 mu m, and the water content is less than 1%.
In the preferred embodiment of the present invention, the calcination temperature is 300-700 deg.C, and the calcination time is 0.5-4 h.
Under the calcination temperature and the calcination time, the red mud and the desulfurized fly ash can fully and completely react.
In the preferred embodiment of the present invention, the red mud is a mixture of red mud produced by any or two methods of bayer process red mud and sintering process red mud;
preferably, the red mud is bayer process red mud;
more preferably, the iron grade TFe of the red mud is 30-60%.
The method provided by the invention is suitable for Bayer process red mud and sintering process red mud, wherein the recovery effect of the Bayer process red mud is optimal. In the Bayer process red mud in the prior art, the iron grade TFe is 30-60%, and the higher the iron grade TFe is, the higher the recovery value is, and the higher the income is. In addition, the red mud also comprises the following components in percentage by weight: al (Al)2O310～45％、SiO25～15％、Na2O 1～10％、TiO21～10％。
In a preferred embodiment of the present invention, the method further comprises controlling the water content in the red mud to be 25-35%, and if the water content in the raw red mud is higher than the above range, drying or plate-and-frame filter pressing the red mud is required. Therefore, the water content is controlled, the subsequent calcination time can be effectively shortened, and the production cost is saved.
In other embodiments, the calcined product may be optionally recycled by another manufacturer.
In a preferred embodiment of the present invention, the method further comprises grinding the calcined product, and magnetically separating the ground mixture to obtain iron micropowder and residue;
preferably, the ratio of the amount of the mixture with fineness less than 0.074mm to the total mixture after grinding is 70-95%.
The product iron micropowder after grinding can be annularly arranged on the surface of the residue in a granular shape, thereby being beneficial to the subsequent magnetic separation and recovery of the iron micropowder. The grinding time is 5-30 min. The control of the grinding fineness is beneficial to recovering the iron micro powder to the maximum extent, and if the grinding fineness is too large, the iron micro powder is difficult to adsorb, and the recovery rate is reduced.
In the preferred embodiment of the present invention, the magnetic separation strength is 40 kA.m-1-200kA·m-1. Under the strength of the magnetic separation, the iron recovery rate of 50-95% can be realized. The grade of iron in the obtained iron micro-powder is related to the grade of iron in the raw red mud, and the higher the grade of iron in the raw red mud is, the higher the grade of iron in the obtained iron micro-powder is. Preferably, the grade of iron in the iron micro powder recovered by the method provided by the invention is 50-90%.
The iron micro powder obtained by the reaction mainly contains ferroferric oxide, and also contains components such as pig iron, ferric silicate, silicate and the like.
In a preferred embodiment of the present invention, the method further comprises crushing the red mud before calcination to a particle size of less than 4 mm.
The red mud is crushed in advance to obtain the red mud with the particle size of less than 4mm, so that the reaction specific surface area of the red mud and the desulfurization ash can be increased, and the recovery rate of the ferric oxide in the red mud is improved.
kinds of stuffing prepared from the residue after magnetic separation of the calcined product prepared by the above method, and the stuffing can be used for building, coal mine backfill and other applications.
cementing material, which comprises filler and auxiliary material, wherein the auxiliary material is at least of cement, slag, fly ash, steel slag and desulfurized gypsum, the mass ratio of the cement in the cementing material is 10-30%, the mass ratio of the slag and the steel slag in the cementing material is less than 60%, the mass ratio of the fly ash in the cementing material is less than 20%, and the mass ratio of the desulfurized gypsum in the cementing material is less than 20%.
After the iron micro powder is recovered by magnetic separation, the residual residue can be used for preparing the cementing material, and corresponding auxiliary materials can be added according to the application of the cementing material to be prepared.
A process for preparing the cementing material includes such steps as mixing filler with auxiliary materials, and grinding.
The prepared cementing material can be used for repairing mines, treating heavy metals and treating sludge, and the iron micro powder obtained by magnetic separation can be used in the fields of iron and steel smelting and the like.
The invention has the following beneficial effects:
the invention provides methods for synergistically recovering red mud and desulfurization ash, which utilize the catalytic oxidation characteristic of iron oxide in the red mud and the reduction characteristic of calcium sulfite in the desulfurization ash, and oxidize the calcium sulfite into calcium sulfate by the iron oxide through calcination, thereby not only realizing the modification of the desulfurization ash, but also realizing the reduction of hematite in the red mud into magnetite, and being beneficial to the subsequent recovery treatment and reutilization of the magnetite.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.
FIG. 1 is a process flow for the synergistic recovery of red mud and desulfurized fly ash provided by the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
The features and properties of the present invention are described in further detail in in conjunction with the examples below.
Example 1
The red mud of the embodiment is Bayer process red mud, and detection shows that the iron grade TFe in the Bayer process red mud is 50 percent, and the red mud additionally contains the following components in percentage by weight2O320％、SiO215％、Na2O 5％、TiO210％。
CaO and Ca (OH) in desulfurized fly ash2The sum of the mass percentages is 40 percent, CaSO350 percent of mass percentage content and the balance of impurities, the granularity is less than 45 mu m, and the moisture is less than 1 percent.
The method for synergistically recovering the red mud and the desulfurized fly ash comprises the following steps:
(1) and carrying out plate-and-frame filter pressing on the Bayer process red mud until the water content is 25%. And crushing the Bayer process red mud subjected to filter pressing by a crusher until the particle size is less than 4 mm.
(2) The crushed red mud and the desulfurized fly ash are mixed by a metering pump according to the mass ratio of 3: 1.
(3) And (3) feeding the well-mixed mixture to a rotary kiln to be roasted for 3 hours at the temperature of 600 ℃.
(4) After roasting, naturally cooling to room temperature, and sending the mixture to a vertical mill for grinding for 30min, wherein the ratio of the fineness of the ground mixture smaller than 0.074mm to the total mixture is 95%.
(5) After grinding, conveying the materials into a magnetic separator, and controlling the magnetic separation strength to be 200 kA.m-1The grade of iron in the obtained iron micro powder is 80 percent, and the recovery rate of iron is 90 percent.
(6) And conveying the rest materials into a storage bin, and finally performing compatible grinding on powder in the storage bin and slag to prepare the cementing material. The mass ratio of the powder to the slag is set to be 4: 1.
Example 2
The red mud of the embodiment is Bayer process red mud, and detection shows that the iron grade TFe in the Bayer process red mud is 60 percent, and the red mud additionally contains the following components in percentage by weight2O330％、SiO25％、Na2O 3％、TiO22％。
CaO and Ca (OH) in desulfurized fly ash2The sum of the mass percentages is 30 percent, CaSO340 percent of mass percentage content and the balance of impurities, the granularity is less than 45 mu m, and the moisture is less than 1 percent.
The method for synergistically recovering the red mud and the desulfurized fly ash comprises the following steps:
(1) and carrying out plate-and-frame filter pressing on the Bayer process red mud until the water content is 30%. And crushing the Bayer process red mud subjected to filter pressing by a crusher until the particle size is less than 4 mm.
(2) The crushed red mud and the desulfurized fly ash are mixed by a metering pump according to the mass ratio of 3: 1.
(3) And (3) delivering the well-mixed mixture to a rotary kiln to be roasted for 3h at 700 ℃.
(4) After roasting, naturally cooling to room temperature, and sending the mixture to a vertical mill for grinding for 30min, wherein the ratio of the fineness of the ground mixture smaller than 0.074mm to the total mixture is 95%.
(5) After grinding, conveying the materials into a magnetic separator, and controlling the magnetic separation strength to be 200 kA.m-1The grade of iron in the obtained iron micro powder is 90 percent, and the recovery rate of iron is 95 percent.
(6) And conveying the rest materials into a storage bin, and finally performing compatible grinding on the powder in the storage bin and the steel slag to prepare the cementing material. The mass ratio of the powder to the steel slag is set to be 5: 1.
Example 3
The red mud of the embodiment is Bayer process red mud, and detection shows that the iron grade TFe in the Bayer process red mud is 60 percent, and the red mud additionally contains the following components in percentage by weight2O315％、SiO215％、Na2O 5％、TiO25 percent. The particle size of the red mud raw material is 2-6mm, andthe water content is less than 20%.
CaO and Ca (OH) in desulfurized fly ash2The sum of the mass percentages is 30 percent, CaSO3The mass percentage content is 60 percent, the rest is impurities, the granularity is less than 45 mu m, and the moisture is less than 1 percent.
The method for synergistically recovering the red mud and the desulfurized fly ash comprises the following steps:
(1) the red mud and the desulfurized fly ash are mixed by a metering pump according to the mass ratio of 3: 1.
(2) And (3) feeding the well-mixed mixture to a rotary kiln to be roasted for 3 hours at the temperature of 600 ℃.
(3) After the roasting is finished, naturally cooling to room temperature to obtain a mixture.
The mixture can be used for iron powder recovery in downstream enterprises.
Example 4
The red mud of the embodiment is Bayer process red mud, and the detection proves that the iron grade TFe in the Bayer process red mud is 30 percent, and the red mud additionally contains the following components in percentage by weight2O345％、SiO215％、Na2O 5％、TiO25 percent. The particle size of the red mud raw material is 2-6mm, and the water content is lower than 20%.
CaO and Ca (OH) in desulfurized fly ash2The sum of the mass percentages is 30 percent, CaSO3The mass percentage content is 60 percent, the rest is impurities, the granularity is less than 45 mu m, and the moisture is less than 1 percent.
The preparation method of the cementing material comprises the following steps:
(1) the red mud and the desulfurized fly ash are mixed by a metering pump according to the mass ratio of 3: 1.
(2) And (3) feeding the well-mixed mixture to a rotary kiln to be roasted for 3 hours at the temperature of 600 ℃.
(3) After roasting, naturally cooling to room temperature, and sending the mixture to a vertical mill for grinding for 30min, wherein the ratio of the fineness of the ground mixture smaller than 0.074mm to the total mixture is 95%.
(4) After grinding, conveying the materials into a magnetic separator, and controlling the magnetic separation intensity to be 150 kA.m-1The grade of iron in the obtained iron micro powder is 50 percent,the iron recovery rate is 60%.
(5) And conveying the residual residues into a storage bin, and finally performing compatibility grinding on powder in the storage bin and cement to prepare the cementing material. The mass ratio of the powder to the auxiliary materials is set to be 5: 1.
Comparative example
Compared with the embodiment 1, the difference is that the iron grade TFe of the red mud is 10%, the other steps are the same, the iron grade in the prepared iron micro powder is 50.3%, and the iron recovery rate is 55.6%.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1, methods for synergistically recovering red mud and desulfurized fly ash, characterized by comprising the step of calcining the red mud and desulfurized fly ash after mixing them.
2. The method according to claim 1, wherein the mass ratio of the red mud to the desulfurized fly ash in the method is 2-6: 1;
preferably, the mass ratio of the red mud to the desulfurized fly ash in the method is 3: 1.
3. The method as claimed in claim 1, wherein the calcination temperature is 300-700 ℃ and the calcination time is 0.5-4 h.
4. The method according to claim 1, wherein the red mud is a mixture of red mud produced by any or both of bayer process red mud and sintering process red mud;
preferably, the red mud is bayer process red mud;
more preferably, the iron grade TFe of the red mud is 30-60%;
more preferably, the red pigmentThe mud also comprises the following components in percentage by weight: al (Al)2O310～45％、SiO25～15％、Na2O 1～10％、TiO21～10％。
5. The method according to claim 1, further comprising pulverizing the calcined product, and magnetically separating the pulverized mixture to obtain fine iron powder and residue;
preferably, the ratio of the mixture with fineness less than 0.074mm to the total mixture after grinding is 70-95%,
preferably, the magnetic separation strength is 40 kA.m-1-200kA·m-1。
6. The method according to claim 1, wherein CaO and Ca (OH) in the desulfurized fly ash2The sum of the mass percentages of the components is 20-40%, and the content of CaSO3The mass percentage content is 30-60%, the particle size of the desulfurization ash is less than 45 mu m, and the moisture content is less than 1%.
7. The method according to claim 1, further comprising crushing the red mud before calcination to a particle size of less than 4 mm.
8, kinds of stuffing, characterized in that the stuffing is prepared from residue after magnetic separation of calcined product prepared by the method of any of claims 1-7.
The cementing material, characterized in that, it includes the filler and auxiliary material of claim 8, the auxiliary material is at least of cement, slag, fly ash, steel slag and desulfurized gypsum, the mass ratio of cement in the cementing material is 10-30%, the mass ratio of slag and steel slag in the cementing material is less than 60%, the mass ratio of fly ash in the cementing material is less than 20%, and the mass ratio of desulfurized gypsum in the cementing material is less than 20%.
10, method for preparing the gelled material of claim 9, wherein the method comprises the steps of mixing and grinding the filler and the auxiliary materials to obtain the gelled material.
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| CN111285406A (en) * | 2020-02-14 | 2020-06-16 | 北京科技大学 | Method for co-recycling alumina red mud and semi-dry desulfurization ash |
| CN111321290A (en) * | 2020-04-01 | 2020-06-23 | 上海应用技术大学 | Comprehensive utilization method of red mud and desulfurized fly ash |
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