CN113651295A - Method for preparing sulfuric acid by treating semidry desulfurization ash and high-sulfur iron material through sintering process - Google Patents
Method for preparing sulfuric acid by treating semidry desulfurization ash and high-sulfur iron material through sintering process Download PDFInfo
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- CN113651295A CN113651295A CN202110852822.2A CN202110852822A CN113651295A CN 113651295 A CN113651295 A CN 113651295A CN 202110852822 A CN202110852822 A CN 202110852822A CN 113651295 A CN113651295 A CN 113651295A
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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
- C01B17/48—Sulfur dioxide; Sulfurous acid
- C01B17/50—Preparation of sulfur dioxide
- C01B17/501—Preparation of sulfur dioxide by reduction of sulfur compounds
- C01B17/506—Preparation of sulfur dioxide by reduction of sulfur compounds of calcium sulfates
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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
- C01B17/48—Sulfur dioxide; Sulfurous acid
- C01B17/50—Preparation of sulfur dioxide
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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
- 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
- C22B1/14—Agglomerating; Briquetting; Binding; Granulating
- C22B1/16—Sintering; Agglomerating
Abstract
The invention discloses a method for preparing sulfuric acid by treating semi-dry desulfurized ash and high-sulfur iron materials by a sintering process. The method realizes the full-component resource recovery of the semi-dry desulfurization ash and the efficient utilization of the high-sulfur iron material, sulfur dioxide flue gas generated in the sintering process is concentrated in the middle of the sintering machine for preparing sulfuric acid, and the sulfur dioxide content of flue gas generated in the rest parts of the sintering machine is low, so that the flue gas after acid preparation can meet the emission requirement after being denitrated.
Description
Technical Field
The invention relates to a method for treating semi-dry desulfurized fly ash, in particular to a method for preparing sulfuric acid by using an iron ore sintering process to cooperatively perform resource treatment on semi-dry desulfurized fly ash, belonging to the technical field of solid waste treatment.
Background
Currently, the flue gas desulfurization technology mainly includes a wet desulfurization technology, a dry desulfurization technology and a semi-dry desulfurization technology. Compared with the former technology, the dry and semi-dry desulphurization technology has the advantages of high desulphurization efficiency, short process flow, lower investment, small occupied area and the like. The semi-dry desulphurization process has obvious advantages and is widely applied to the industries of ferrous metallurgy, thermal power generation and the like.
The desulfurized fly ash produced by the semi-dry desulfurization process mainly comprises the following components: free calcium oxide, calcium sulfite, calcium hydroxide, calcium sulfate, a small amount of calcium carbonate and the like. The semi-dry desulfurized fly ash is alkaline as a whole, and free calcium oxide is easy to absorb water and expand; the components of calcium sulfite, calcium hydroxide and calcium carbonate are easily decomposed by heating, have instability and the like, and belong to solid hazardous waste which is difficult to treat.
At present, the semi-dry desulfurized fly ash is mainly applied to the aspect of cement auxiliary materials at home and abroad. The semi-dry desulfurized fly ash has higher sulfur content, contains more free calcium oxide and continuously generates Ca (OH) in the long-term hydration process2The volume is expanded continuously, which affects the stability of use, and the cement can not be used directly or the use amount is less, so that the resource utilization is limited. Most of the desulfurized ash can be treated only by piling and burying, which not only damages the environment, but also occupies land resources. Meanwhile, a large amount of resources such as calcium, sulfur and the like in the semidry desulfurization ash are not utilized massively, so that the waste of resources is caused.
Therefore, a technology for comprehensively utilizing the semi-dry desulfurized fly ash is sought, so that the problem of on-site resource utilization of the desulfurized fly ash is urgently solved.
Disclosure of Invention
The invention aims to provide a method for realizing resource utilization of semi-dry desulfurized ash by treating the semi-dry desulfurized ash in the iron ore sintering process, aiming at solving the technical problem that the semi-dry desulfurized ash is difficult to treat and comprehensively utilized in the prior art, the method utilizes the semi-dry desulfurized ash to simultaneously provide a calcium source and a sulfur source, takes solid fuel as a carbon source to simultaneously provide a heat source for production and promote the decomposition of calcium sulfate, and is added with a high-sulfur iron material to provide an iron source.
In order to achieve the technical purpose, the invention provides a method for preparing sulfuric acid by treating semi-dry desulfurization ash and high-sulfur iron materials through a sintering process, which comprises the steps of blending, uniformly mixing and granulating the semi-dry desulfurization ash, the high-sulfur iron materials, quick lime and solid fuel to obtain a ball material, and sequentially distributing, igniting and sintering the ball material to obtain a sintered material; wherein, the flue gas with high sulfur dioxide concentration generated in the middle of the sintering machine is used for preparing sulfuric acid in the sintering process.
According to the technical scheme, the semi-dry desulfurized fly ash, the high-sulfur iron material, the quick lime and the solid fuel are matched to utilize the iron ore sintering process to complete the high-temperature reaction among various raw materials, so that the sulfur and calcium in the semi-dry desulfurized fly ash and the sulfur in the high-sulfur iron material are fully recovered and recycled. During sintering, the semidry desulfurized fly ash is used as a calcium source and a sulfur source, calcium sulfite, calcium oxide, calcium hydroxide and calcium carbonate in the semidry desulfurized fly ash are easy to participate in reaction in high-temperature reaction, and calcium sulfate with better stability can promote conversion under the action of a carbonaceous reducing agent and a high-sulfur iron material, so that most of sulfur in the semidry desulfurized fly ash enters flue gas in the form of sulfur dioxide, and calcium in the semidry desulfurized fly ash participates in the generation of calcium ferrite, so that a qualified iron ore sintering material is obtained. The single high-sulfur iron material is difficult to obtain high-sulfur dioxide flue gas meeting the requirement of preparing sulfuric acid in the calcining process, the concentration of sulfur dioxide in the flue gas is greatly improved after the flue gas is matched with semi-dry desulfurization ash for high-temperature solid-phase reaction so as to meet the requirement of preparing sulfuric acid, andiron oxide generated in the process of calcining the high-sulfur iron material can promote the conversion of components in the semi-dry desulfurization ash. The solid fuel not only plays a role in heat supply, but also plays a role in weak reduction promotion in key, and is beneficial to the conversion of calcium sulfate and the like. The quicklime is used as a calcium source and a binder on one hand, and can be used for absorbing SO generated in a combustion zone at the head position of a sintering machine on the other hand2SO in head flue gas2The concentration is reduced to 35mg/m3In the following, the flue gas desulfurization treatment is not required, and the wet material carries adsorbed SO2After entering the middle part of the sintering machine, the SO in the middle flue gas is improved2The concentration of (b) is favorable for preparing sulfuric acid.
As a preferred scheme, the main components of the semi-dry desulfurization ash comprise calcium sulfite, calcium sulfate, calcium oxide, calcium hydroxide and calcium carbonate. The semi-dry desulfurized fly ash is common solid waste in the industry, such as a byproduct of semi-dry desulfurization of flue gas of a steel plant or a power plant by using a calcareous desulfurizer.
As a preferable scheme, the sulfur content of the high-sulfur iron material is not less than 0.2%. The high-sulfur iron material can be selected from natural iron ore or secondary iron-containing material with higher sulfur content.
As a preferable mode, the fixed carbon content of the solid fuel is more than 75% by mass. The solid fuel can be at least one of coke powder, coal or biomass fuel.
As a preferable scheme, the CaO content of the quicklime is not lower than 82% by mass, and the activity is not lower than 250 mL. The quicklime is generally fully digested and then mixed with ingredients and granulated.
As a preferable scheme, the principle of the ingredients is measured by taking the total mass of the semi-dry desulfurized fly ash, the high-sulfur iron material and the quick lime as 100 percent, and the following requirements are met: the mass percentage content of the quicklime is 3-5%; the mass percentage content of the semi-dry desulfurization ash is 15-50 percent; the mass percentage content of the high-sulfur iron material is 45-82 percent; the mass of the solid fuel is 4-8% of the total mass of the semi-dry desulfurized fly ash, the high-sulfur iron material and the quicklime. According to the preferable proportioning principle, the semi-dry desulfurized fly ash has high occupation ratio, and is matched with a high-sulfur iron material and quick lime according to a proper proportion to carry out high-temperature reaction, calcium sulfite, calcium sulfate and the like in the semi-dry desulfurized fly ash almost complete the reaction, most of sulfur is transferred to flue gas in the form of sulfur dioxide and is enriched in the middle flue gas of a sintering machine to be recovered, the sulfur can be used for preparing acid, calcium becomes an important constituent element of an iron ore sintering material in the form of calcium ferrite and the like, and the resource utilization of sulfur is realized.
As a preferable scheme, the average particle size of the granules is 4-6 mm, and the mass percentage content of the-1 mm fraction is not higher than 6%.
As a preferred scheme, the thickness of the cloth is 600-1000 mm.
As a preferable scheme, the middle part of the sintering machine is from the position where the concentration of sulfur dioxide in the flue gas begins to rise to SO2The concentration is reduced to 35mg/m after reaching the maximum value3The middle part of the sintering machine accounts for 35 to 40 percent of the total length of the sintering machine in the area between the positions.
As a preferable scheme, flue gas generated in a region other than the middle part of the sintering machine during sintering is subjected to dust removal treatment, and is subjected to denitration together with flue gas after sulfuric acid preparation and then discharged. The sulfur dioxide content in the flue gas in the area outside the middle part of the sintering machine is low, and the desulfurization treatment is not needed.
As a preferable scheme, the ignition temperature is 1050-1200 ℃, and the time is 1-2 min.
Preferably, the sintering speed is 14-20 mm/min. The burning zone gradually moves from the upper part to the lower material layer in the sintering process until the burning process is finished.
The pellet of the invention has over 90% of the sulfur removed as sulfur dioxide to the flue gas during sintering, and the sintered material has very low sulfur content.
The sintering machine is divided into three areas, namely a head area, a middle area and a tail area according to the release rule of sulfur dioxide in the sintering process, wherein the head area is SO in flue gas2The region with non-rising concentration accounts for 40-45% of the total length of the sintering machine; the middle part is flue gas SO2The concentration begins to risePosition to SO2The concentration is reduced to 35mg/m after reaching the maximum value3The area (2) accounts for 35 to 40 percent of the length of the sintering machine; the tail part is the rest tail area and accounts for 15 to 25 percent of the sintering machine. SO in flue gas in the middle of sintering machine2High concentration, and can be directly used for preparing sulfuric acid.
The sintering material is crushed, cooled, screened and screened to obtain qualified sintering material products with the size fraction of more than +5mm and the size fraction of less than-5 mm, and the qualified sintering material products are returned to the sintering process as return ores for recycling.
The process for preparing the sulfuric acid is a common process in the industry, and particularly relates to a process for preparing high SO2And (4) dedusting, washing and catalytically converting the flue gas to obtain industrial sulfuric acid.
The invention takes semidry desulfurization ash, high-sulfur iron material, quicklime and solid fuel as raw materials, and the raw materials are mixed, evenly mixed and granulated to obtain the pellet. And then, distributing the pellets on a sintering machine for ignition and sintering, wherein in the sintering process, more than 95% of sulfur in the pellets is removed to flue gas in the form of sulfur dioxide, and the sulfur is enriched to the flue gas in the middle of the sintering machine to obtain the flue gas containing high-concentration sulfur dioxide, and the flue gas is directly used for preparing sulfuric acid.
Compared with the prior art, the technical scheme of the invention has the following beneficial technical effects:
1) the technical scheme of the invention is that the industrial sulfuric acid is prepared by using semi-dry desulfurized fly ash, high-sulfur iron material, quicklime and solid fuel as main raw materials, the utilization ratio of the semi-dry desulfurized fly ash is high, and the ratio of the semi-dry desulfurized fly ash in the raw materials is 15-50%. According to the method, calcium sulfite, calcium sulfate and sulfur-containing iron materials in the desulfurized ash are almost reacted through a sintering process, and the generated sulfur dioxide is transferred into flue gas and enriched in the middle flue gas of a sintering machine for recycling, so that the resource utilization of sulfur is realized;
2) the technical scheme of the invention simultaneously solves the problem of utilization of the high-sulfur iron material, and the high-sulfur iron material is treated by conventional sintering because of SO2The concentration can not meet the requirement of acid production, the cost of flue gas desulfurization treatment is high, and in the scheme of the invention, the sulfur in the high-sulfur iron material is recycled and used for producing acid, and the decomposition of calcium sulfate in the desulfurized ash is facilitated, so that mutual promotion is realizedThe function of (1).
3) In the technical scheme of the invention, a small amount of by-product calcium sulfide generated in the high-temperature combustion zone can be oxidized into CaO and SO in the cooling zone2Ensure that the sulfur is converted into SO more completely2And the sulfur enters the flue gas, so that the recovery rate of sulfur is further improved.
4) In the technical scheme of the invention, SO generated by a combustion zone at the head part of the sintering machine2The wet material belt area of the lower material layer is absorbed by calcium hydroxide to promote SO in the head smoke2The concentration is reduced to 35mg/m3In the following, the flue gas desulfurization treatment is not required; SO adsorbed by wet material belt2After entering the middle part of the sintering machine, the SO in the middle flue gas is improved2So that it is advantageous for the production of acid.
5) According to the technical scheme, the flue gas at the head part and the flue gas at the tail part of the sintering machine are dedusted, combined with the flue gas at the middle part of the sintering machine after acid making, and then denitrated together, so that the requirement of flue gas discharge can be met, and the flue gas treatment cost is reduced.
6) According to the technical scheme, calcium oxide generated in the roasting process is combined with ferric oxide to generate calcium ferrite, so that the qualified iron ore sintering material is obtained, and the comprehensive utilization of a calcium source in the desulfurized fly ash is realized.
In conclusion, the method realizes the full component utilization of calcium and sulfur elements in the semidry desulfurization ash, realizes the large and harmless treatment of the desulfurization ash, and has better social benefit, environmental protection benefit and economic benefit.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, rather than all embodiments, and all other embodiments obtained by those skilled in the art without any creative work based on the embodiments of the present invention belong to the protection scope of the present invention.
Example 1
Firstly, taking semi-dry desulfurized fly ash with 12.9 percent of sulfur by mass, high-sulfur iron material with 0.2 percent of sulfur by mass and CaO by mass in a power plantQuicklime with the content of 82 percent and the activity of 250mL respectively accounts for 45 percent, 51 percent and 4 percent by mass, and coke powder with the fixed carbon content of 80 percent is externally added for 5 percent, and then the mixture is mixed and evenly granulated to prepare 5mm pellets. And (3) sequentially distributing the ball materials, wherein the thickness of the cloth is 800 mm. After the material distribution is finished, igniting under the surface of the mixture, wherein the ignition temperature is 1050 ℃ and the time is 2 min. After the fuel on the surface of the material layer is ignited and combusted, the material layer enters a sintering stage, the sintering speed is 16mm/min, and the combustion zone gradually moves from the upper part to the lower material layer until the combustion process is finished to obtain a sintered material; the high-concentration sulfur dioxide generated in the sintering process is released to the middle part of the sintering machine in a centralized way, and finally the SO in the middle flue gas of the sintering machine2The concentration is 3.8%, and the method can be used for preparing industrial sulfuric acid.
Example 2
Firstly, taking semi-dry desulfurized ash with 13.1 percent of sulfur by mass, high-sulfur iron material with 0.9 percent of sulfur by mass and quicklime with 88 percent of CaO by mass and activity of 280mL in a certain steel plant, respectively taking 50 percent, 45 percent and 5 percent of sulfur by mass and additionally adding 8 percent of anthracite with 75 percent of fixed carbon by mass, mixing the materials, and uniformly granulating to prepare pellets with the diameter of 4 mm. And (3) sequentially distributing the ball materials, wherein the thickness of the cloth is 600 mm. After the material distribution is finished, igniting under the surface of the mixed material, wherein the ignition temperature is 1100 ℃, and the time is 2 min. After the fuel on the surface of the material layer is ignited and combusted, the material layer enters a sintering stage, the sintering speed is 20mm/min, and the combustion zone gradually moves from the upper part to the lower material layer until the combustion process is finished to obtain a sintered material; the high-concentration sulfur dioxide generated in the sintering process is released to the middle part of the sintering machine in a centralized way, and finally the SO in the middle flue gas of the sintering machine2The concentration is 4.3%, and the method can be used for preparing industrial sulfuric acid.
Example 3
Firstly, taking semi-dry desulfurized ash with 12.9 percent of sulfur mass percentage in a certain steel plant, high-sulfur iron material with 2.3 percent of sulfur mass percentage and quicklime with 90 percent of CaO mass percentage and activity of 290ml, respectively taking 15 percent, 82 percent and 3 percent of the semi-dry desulfurized ash, externally reinforcing 4 percent of coke powder with 80 percent of carbon mass percentage, mixing the materials, uniformly granulating to obtain 6mm small coke powderA ball. And (3) sequentially distributing the ball materials, wherein the thickness of the cloth is 1000 mm. After the material distribution is finished, igniting under the surface of the mixed material, wherein the ignition temperature is 1200 ℃ and the time is 1 min. After the fuel on the surface of the material layer is ignited and combusted, the material layer enters a sintering stage, the sintering speed is 14mm/min, and the combustion zone gradually moves from the upper part to the lower material layer until the combustion process is finished to obtain a sintered material; the high-concentration sulfur dioxide generated in the sintering process is released to the middle part of the sintering machine in a centralized way, and finally the SO in the middle flue gas of the sintering machine2The concentration is 4.0%, and the method can be used for preparing industrial sulfuric acid.
The above description is only a preferred embodiment of the present invention, and the protection scope of the present invention is not limited to the above-described embodiments. Modifications and variations that may occur to those skilled in the art without departing from the spirit and scope of the invention are to be considered as within the scope of the invention.
Claims (10)
1. A method for preparing sulfuric acid by treating semidry desulfurization ash and high-sulfur iron materials by a sintering process is characterized by comprising the following steps: blending, uniformly mixing and granulating semi-dry desulfurized fly ash, a high-sulfur iron material, quicklime and solid fuel to obtain a ball material, and sequentially distributing, igniting and sintering the ball material to obtain a sintered material; wherein, the flue gas with high sulfur dioxide concentration generated in the middle of the sintering machine is used for preparing sulfuric acid in the sintering process.
2. The method for preparing sulfuric acid by treating semidry desulfurized ash and high-sulfur iron materials through sintering process according to claim 1, characterized in that: the main components of the semi-dry desulfurization ash comprise calcium sulfite, calcium sulfate, calcium oxide, calcium hydroxide and calcium carbonate.
3. The method for preparing sulfuric acid by treating semidry desulfurized ash and high-sulfur iron materials through sintering process according to claim 1, characterized in that: the sulfur content of the high-sulfur iron material is not less than 0.2%.
4. The method for preparing sulfuric acid by treating semidry desulfurized ash and high-sulfur iron materials through sintering process according to claim 1, characterized in that: the solid fuel has a fixed carbon mass percent content of greater than 75%.
5. The method for preparing sulfuric acid by treating semidry desulfurized ash and high-sulfur iron materials through sintering process according to claim 1, characterized in that: the CaO content of the quicklime is not lower than 82% by mass, and the activity is not lower than 250 mL.
6. The method for preparing sulfuric acid by treating semidry desulfurized ash and high-sulfur iron materials through a sintering process according to any one of claims 1 to 5, characterized by comprising the following steps:
the principle of batching, with the total mass of semi-dry desulfurization ash, high-sulfur iron material and quick lime as 100% measurement, satisfies:
the mass percentage content of the quicklime is 3-5%;
the mass percentage content of the semi-dry desulfurization ash is 15-50 percent;
the mass percentage content of the high-sulfur iron material is 45-82 percent;
the mass of the solid fuel is 4-8% of the total mass of the semi-dry desulfurized fly ash, the high-sulfur iron material and the quicklime.
7. The method for preparing sulfuric acid by treating semidry desulfurized ash and high-sulfur iron materials through sintering process according to claim 1, characterized in that: the average particle size of the granules is 4-6 mm, and the mass percentage content of the-1 mm fraction is not higher than 6%.
8. The method for preparing sulfuric acid by treating semidry desulfurized ash and high-sulfur iron materials through sintering process according to claim 1, characterized in that: the thickness of the cloth is 600-1000 mm.
9. The method for preparing sulfuric acid by treating semidry desulfurized ash and high-sulfur iron materials through sintering process according to claim 1, characterized in that: the middle part of the sintering machine is from the position where the concentration of sulfur dioxide in the flue gas begins to rise to SO2The concentration is reduced to the maximum value35mg/m3The middle part of the sintering machine accounts for 35 to 40 percent of the total length of the sintering machine in the area between the positions.
10. The method for preparing sulfuric acid by treating semidry desulfurized ash and high-sulfur iron materials through sintering process according to claim 1, characterized in that: and in the sintering process, flue gas generated by an area except the middle part of the sintering machine is subjected to dust removal treatment, and is subjected to denitration together with flue gas after sulfuric acid preparation and then discharged.
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