CN110950338B - Method for capturing carbon dioxide in converter flue gas and coproducing NPCC (neutral carbon dioxide) by closed cycle of converter steel slag and steelmaking wastewater - Google Patents
Method for capturing carbon dioxide in converter flue gas and coproducing NPCC (neutral carbon dioxide) by closed cycle of converter steel slag and steelmaking wastewater Download PDFInfo
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Abstract
A method for capturing carbon dioxide in converter flue gas and co-producing NPCC by closed cycle of converter steel slag and steelmaking wastewater is carried out according to the following steps: (1) grinding the converter steel slag; (2) Placing steel slag powder into a rotary packed bed, adding steel-making wastewater to carry out leaching reaction, and filtering to obtain leaching liquid; (3) Heating the leaching solution to 30-80 ℃, introducing converter flue gas, stirring for carbonization reaction, washing and drying the filtered solid phase to prepare nano calcium carbonate, and returning the liquid phase for recycling. The method provided by the invention realizes the synergistic treatment effect of converter slag, cold rolling wastewater and converter waste gas, and simultaneously coproduces the high added value product nano calcium carbonate.
Description
Technical Field
The invention belongs to the technical field of metallurgical waste utilization and environmental protection, and particularly relates to a method for co-producing NPCC by capturing carbon dioxide in converter flue gas in a closed cycle manner through converter steel slag-steelmaking wastewater.
Background
With the development of the steel industry, as the steel productivity further increases, CO 2 The discharge amount of the waste water is increased year by year, and the waste water brings serious harm to the environment. At present, main strategies for carbon dioxide emission reduction include ocean landfill, geological storage and mineral carbonization; both marine landfills and geological sequestration, while having the ability to sequester large amounts of carbon dioxide, are not highly safe, with the risk of carbon dioxide leakage, whereas mineral carbonization has incomparable advantages over the former in terms of stability and safety. If the waste (such as steel slag) of a steel mill is used as a carbon capture carrier, the method has more efficient emission reduction effect, can realize low cost, and can realize green carbon capture and simultaneously realize bulk utilization of the steel slag as a building material.
A large amount of industrial solid waste steel slag is generated in the steelmaking process, the steel slag contains a large amount of calcium oxide, and the steel slag yield is rich; because the steel slag particles are small (in the level of common millimeter), the steel slag carbonization has better carbonization dynamics effect, and provides theoretical feasibility for realizing large-scale carbon dioxide capture for mineral carbonization; at present, the mineral carbonization method has two types of dry carbonization and wet carbonization, and compared with the steel slag dry carbonization, the steel slag wet carbonization has the advantages of low cost, good carbonization effect, strong operation controllability and the like; if the fresh water is adopted as the mass transfer medium for steel slag carbonization, the water consumption is huge, the carbonization cost is higher, and a steel mill has a large amount of steelmaking wastewater, if the steelmaking wastewater is adopted as the mass transfer medium for steel slag wet carbonization, the steelmaking wastewater has the inherent advantage, and the steelmaking wastewater is used for steel slag wet carbonization, so that the mass transfer kinetics of carbon dioxide can be effectively improved, the steel slag carbonization depth is improved, and the low-cost desalting effect of the steelmaking wastewater can be realized. Slag-steelmaking wastewater CO capture 2 The new circulation process realizes carbon capture, and simultaneously, the stability problem of large-scale utilization of steel slag as a building material and the desalting problem in the steelmaking wastewater circulation treatment process are cooperatively considered.
The steel slag carbonization technology not only can solidify a large amount of CO 2 And can also realize the effective utilization of secondary resources such as steel slag, waste water and the like. Researchers propose the idea of leaching calcium element in steel slag with ammonium salt and using it to prepare calcium carbonate; the invention of application number 201811161199.0 discloses a method for preparing light calcium carbonate by utilizing steel slag, which adopts microwaves to carry out irradiation pretreatment on the steel slag, and has the advantages that a leaching agent can be recycled, high-value-added high-purity calcium carbonate can be produced, but the method has the advantages of larger energy consumption, low leaching rate of calcium in the steel slag, larger granularity of the prepared calcium carbonate and no consideration of application and treatment of wastewater; so far, few patent and non-patent documents at home and abroad directly adopt metallurgical waste residue and waste water to directly cooperatively couple mineralize and seal CO 2 Report of preparation of nano calcium carbonate.
Disclosure of Invention
In view of the above-mentioned deficiencies in the art of existing metallurgical waste treatment and utilization, the present invention provides a rotary furnaceMethod for capturing carbon dioxide in converter flue gas and CO-producing NPCC by closed cycle of steel slag-steelmaking wastewater, and capturing solidified CO by using converter steel slag, steelmaking wastewater and converter flue gas 2 Nano calcium carbonate is prepared, under the action of ions contained in wastewater, the leaching rate of calcium ions is increased, and CO is improved 2 The mass transfer rate of the converter slag is matched with the steelmaking wastewater and the converter flue gas to realize the secondary utilization of the converter slag and reduce CO 2 And simultaneously preparing high-purity nano calcium carbonate (NPCC).
The method of the invention comprises the following steps:
1. crushing and grinding converter steel slag to a grain size less than or equal to 100 mu m to prepare steel slag powder;
2. placing steel slag powder into a rotary packed bed, adding steel-making wastewater into the rotary packed bed for leaching reaction, wherein the ratio of the steel slag powder to the steel-making wastewater is 1 (50-100) kg/L according to the solid-to-liquid ratio, the leaching reaction time is 20-200 min, and filtering and separating materials after the reaction is finished to obtain a liquid phase which is a leaching solution rich in calcium ions;
3. heating the leaching solution to 30-80 ℃, then introducing converter flue gas into the leaching solution, stirring for carbonization reaction, wherein the stirring speed is 500-1000 rpm, the carbonization reaction time is 30-60 min, filtering and separating materials after the reaction is finished, washing and drying the obtained solid phase to prepare nano calcium carbonate, and returning the obtained liquid phase to the step 2 for recycling as steelmaking wastewater.
The converter steel slag contains CaO 30-60 wt% and SiO 2 17～42％，Fe 2 O 3 0.8～18％，MgO 0.1～13％，Al 2 O 3 3～5％，SO 3 0～1.2％，P 2 O 5 1.2～2.8％，CaCO 3 0～2.5％。
The concentration of each ion in the steelmaking wastewater is Na + 700～900mg/L，K + 200～350mg/L，Ca 2+ 50～300mg/L，Zn 2+ 60～80mg/L，Cl - 1200～1600mg/L，O 4 2- 150～300mg/L，NO 3 - 5～15mg/L，NH 4 + 400-900 mg/L; the pH value of the steelmaking wastewater is 8-13.
The converter flue gas contains 16-30% of CO and 16-30% of CO by volume 2 10～40％、N 2 36～46％、NO x 0～2％。
In the method, the carbonization rate of calcium in the leaching solution is 95-100%.
In the method, the leaching rate of calcium ions in the converter steel slag is 95-99%.
In the method, the ratio of the total volume of the flue gas introduced into the converter to the total mass of the converter steel slag is 270-2390 m 3 /t。
In the step 2, the desalination rate of calcium ions in the obtained liquid phase is 90-99%, and the pH value of the liquid phase is 6.2-7.2.
The granularity of the nano calcium carbonate is 100-950 nm.
In the method, the yield of the nano calcium carbonate is 0.48-0.96 t/t converter steel slag.
In the step 3, CO in the converter flue gas 2 The trapping rate of the catalyst is 90-99%.
The steelmaking wastewater is cold rolling wastewater.
In the step 2, the main reaction equation of the reaction is:
2CaO·SiO 2 (s)+4NH 4 + (aq)+4Cl - (aq)→2Ca + +4Cl - (aq)+2H 2 O+SiO 2 (s)↓+4NH 3 (aq) (1)
CaO(s)+2NH 4 + (aq)+2Cl - (aq)→Ca 2+ (aq)+H 2 O(l)+2NH 3 (aq)+2Cl - (aq) (2)
CaO(s)+H 2 O(g)＝Ca(OH) 2 (aq) (3)
in the above step 3, the reaction equation is:
4NH 3 (aq)+2CO 2 (aq)+2Ca + (aq)+4Cl - (aq)+4H 2 O(l)→2CaCO 3 (s)↓+4NH 4 + +4Cl - (aq) (4)
the method of the invention has the following characteristics:
1. has higher leaching rate of calcium ions; ammonium ions and chloride ions contained in the adopted steelmaking cold rolling wastewater can promote the leaching of calcium ions, so that the leaching rate of the calcium ions is improved, and meanwhile, the concentration of the calcium ions in the leaching solution is also improved by the calcium ions contained in the wastewater;
2. has higher carbonization rate and NPCC yield; the ionic component in the adopted wastewater can greatly promote CO 2 The mass transfer rate of NPCC is improved;
3. the production process is simple and the cost is low; the waste water, waste gas and steel slag of the steelmaking and cold rolling are by-products generated in the steelmaking process, the cost is low, and other catalytic substances are not needed in the reaction process, so that the reaction cost is reduced;
4. the product quality is good; the prepared NPCC has uniform granularity and regular shape; the product has small particle size, no impurity and higher purity;
5. energy conservation and environmental protection; the waste water is subjected to preliminary desalination, and the treated waste gas is solidified due to the carbon dioxide, so that the purity of the carbon monoxide is improved, and the carbon monoxide can be directly returned to a metallurgical process for cyclic application, thereby achieving the effects of energy conservation and environmental protection;
6. secondary utilization of steel slag resources is realized; not only can produce high-quality nano calcium carbonate, but also can realize the aim of bulk utilization of steel slag resources due to the improvement of the stability of the steel slag.
The invention has simple process, low cost and energy consumption, can realize carbon dioxide emission reduction, and can realize secondary resource circulation of steel slag and the like; cold rolling waste water is adopted as CO in the process 2 Mass transfer medium, which is favorable for improving CO in the carbon capture reaction process 2 Mass transfer kinetics, and effectively improves the yield of NPCC. Meanwhile, the treated cold rolling wastewater degrades the hardness of the wastewater due to the deep removal of calcium ions; CO 2 The concentration of CO in the solidified waste gas is obviously improved, and the waste gas is returned to the metallurgical process flow as a reducing atmosphere; the method realizes the synergistic treatment effect of converter slag, cold rolling wastewater and converter waste gas, and simultaneously coproduces the high added value product nano calcium carbonate.
Drawings
FIG. 1 is a schematic flow chart of a method for capturing carbon dioxide in converter flue gas and co-producing NPCC by closed cycle of converter steel slag and steelmaking wastewater in an embodiment of the invention;
FIG. 2 is a schematic diagram of a device for capturing carbon dioxide in converter flue gas and co-producing NPCC in a closed cycle manner by converter steel slag-steelmaking wastewater in an embodiment of the invention;
in the figure, 1, a wastewater tank, 2, a first water pump, 3, a wastewater pipe, 4, a rotary packed bed, 5, a discharging chamber, 6, a first filter, 7, a leaching liquid pipe, 8, a reactor, 9, an air inlet pipe, 10, an air outlet pipe, 11, an air storage tank, 12, a wastewater circulation pipeline, 13, a second filter, 14, a second water pump, 15, a stirring paddle, 16 and a third water pump.
Detailed Description
The flow of the embodiment of the invention is shown in figure 1.
The structure of the device for capturing carbon dioxide and co-producing NPCC in converter flue gas by closed cycle of converter steel slag-steelmaking wastewater adopted in the embodiment of the invention is shown in figure 2, and the device comprises a wastewater tank 1, a rotary packed bed 4, a reactor 8 and a gas storage tank 11, wherein the bottom of the wastewater tank 1 is communicated with the inlet of a first water pump 2 through a pipeline with a valve, the outlet of the first water pump 2 is communicated with a discharging chamber 5 in the rotary packed bed 4 through a wastewater conduit 3, the discharge port of the rotary packed bed 4 is communicated with the inlet of a first filter 6 through a pipeline with a valve, the filtrate outlet of the first filter 6 is communicated with the inlet of a second water pump 14 through a pipeline with a valve, and the outlet of the second water pump 14 is communicated with the feed inlet of the reactor 8 through a leaching liquid conduit 7; an air outlet pipe 10 is arranged above the reactor 8; the side wall of the reactor 8 is communicated with a gas storage tank 11 through a gas inlet pipe 9, and the gas storage tank 11 is used for storing converter flue gas; the air outlet of the air inlet pipe 9 is positioned at the bottom of the reactor 8; a stirring paddle 15 is arranged in the reactor 8; the bottom of the reactor 8 is provided with a discharge port which is communicated with the inlet of the second filter 13 through a pipeline with a valve; the second filter 13 communicates with the wastewater tank 1 through a wastewater circulation pipe 12, and a third water pump 16 is installed on the wastewater circulation pipe 12.
The converter steel slag adopted in the embodiment of the invention is converter slag produced in a converter workshop, the steelmaking wastewater is cold-rolled wastewater of a steel mill, and the converter flue gas is converter flue gas discharged by the steel mill.
The converter slag adopted in the embodiment of the invention contains 30-60% of CaO and SiO by mass percent 2 17～42％，Fe 2 O 3 0.8～18％，MgO 0.1～13％，Al 2 O 3 3～5％，SO 3 0～1.2％，P 2 O 5 1.2～2.8％，CaCO 3 0～2.5％。
In the embodiment of the invention, the concentration of each ion in the steelmaking wastewater is Na + 700～900mg/L，K + 200～350mg/L，Ca 2 + 50～300mg/L，Zn 2+ 60～80mg/L，Cl - 1200～1600mg/L，SO 4 2- 150～300mg/L，NO 3 - 5～15mg/L，NH 4 + 400-900 mg/L and pH value of 8-13.
The converter flue gas adopted in the embodiment of the invention contains 16-30% of CO by volume percentage, and the CO 2 30～40％，N 2 36～46％，NO x 0～2％。
In the embodiment of the invention, the flow of the flue gas of the transfer furnace is introduced into the reactor according to the flow of 0.5-5L/min.
The water washing in the embodiment of the invention means that the water washing stone filtrate is neutral, and the drying is to remove water by drying under the condition of 120 ℃.
In the embodiment of the invention, the desalination rate of calcium ions in the liquid phase obtained by filtering after leaching is 90-99%, and the pH value of the liquid phase is 6.2-7.2.
In the embodiment of the invention, the yield of the nano calcium carbonate is 0.48-0.96 t/t converter steel slag.
In the embodiment of the invention, CO in the converter flue gas 2 The trapping rate of the catalyst is 90-99%.
In the embodiment of the invention, cold rolling wastewater is selected as steelmaking wastewater.
Example 1
Crushing and grinding converter steel slag to a grain size of 10-40 mu m to prepare steel slag powder;
a device for capturing carbon dioxide in converter flue gas and coproducing NPCC by adopting closed cycle of converter steel slag and steelmaking wastewater; placing steel slag powder into a rotary packed bed, adding steel-making wastewater into the rotary packed bed for leaching reaction, wherein the ratio of the steel slag powder to the steel-making wastewater is 1:50kg/L, the leaching reaction time is 200min, and filtering and separating materials after the reaction is finished to obtain a liquid phase which is a leaching solution rich in calcium ions; the carbonization rate of calcium in the leaching solution is 100%; the leaching rate of calcium ions in the converter slag is 95%;
heating the leaching solution to 30 ℃, then introducing converter flue gas into the leaching solution, stirring for carbonization reaction, wherein the stirring speed is 1000rpm, the carbonization reaction time is 60min, and the ratio of the total volume of the introduced converter flue gas to the total mass of the converter steel slag is 2200m 3 T; filtering and separating the materials after the reaction is finished, washing and drying the obtained solid phase to prepare nano calcium carbonate with the granularity of 100-400 nm; and returning the liquid phase obtained by filtering to the step 2 to be used as steelmaking wastewater for recycling.
Example 2
The process is the same as in example 1, except that:
(1) The grain diameter of the steel slag powder is 40-60 mu m; the ratio of the steel slag powder to the steel-making wastewater is 1:80kg/L, and the leaching reaction time is 100min;
(2) The carbonization rate of calcium in the leaching solution is 98%; the leaching rate of calcium ions in the converter slag is 97%;
(3) Heating the leaching solution to 50 ℃, introducing converter flue gas, stirring at 800rpm for 40min, wherein the ratio of the total volume of the introduced converter flue gas to the total mass of the converter steel slag is 1200m 3 /t；
(4) The granularity of the nano calcium carbonate is 400-600 nm.
Example 3
The process is the same as in example 1, except that:
(1) The grain diameter of the steel slag powder is 60-80 mu m; the ratio of the steel slag powder to the steel-making wastewater is 1:100kg/L, and the leaching reaction time is 20min;
(2) The carbonization rate of calcium in the leaching solution is 95%; the leaching rate of calcium ions in the converter slag is 99%;
(3) Heating the leaching solution to 80 ℃ and introducing converter flue gasStirring speed is 500rpm, carbonization reaction time is 30min, and the ratio of total volume of the flue gas introduced into the converter to total mass of the converter steel slag is 300m 3 /t；
(4) The granularity of the nano calcium carbonate is 600-800 nm.
Claims (4)
1. A method for capturing carbon dioxide in converter flue gas and co-producing NPCC by closed cycle of converter steel slag and steelmaking wastewater is characterized by comprising the following steps:
(1) Crushing and grinding converter steel slag to a grain size less than or equal to 100 mu m to prepare steel slag powder;
(2) Placing steel slag powder into a rotary packed bed, adding steel-making wastewater into the rotary packed bed for leaching reaction, wherein the ratio of the steel slag powder to the steel-making wastewater is 1 (50-100) kg/L according to the solid-to-liquid ratio, the leaching reaction time is 20-200 min, and filtering and separating materials after the reaction is finished to obtain a liquid phase which is a leaching solution rich in calcium ions; the leaching rate of calcium ions in the converter slag is 95-99%;
(3) Heating the leaching solution to 30-80 ℃, then introducing converter flue gas into the leaching solution, stirring for carbonization reaction, wherein the stirring speed is 500-1000 rpm, the carbonization reaction time is 30-60 min, filtering and separating materials after the reaction is finished, washing and drying an obtained solid phase to prepare nano calcium carbonate, and the granularity of the nano calcium carbonate is 100-950 nm; returning the obtained liquid phase to the step 2 to be used as steelmaking wastewater for recycling;
the converter steel slag contains 30-60% of CaO and SiO by weight percent 2 17～42％，Fe 2 O 3 0.8～18％，MgO 0.1～13％，Al 2 O 3 3～5％，SO 3 0～1.2％，P 2 O 5 1.2～2.8％，CaCO 3 0～2.5％；
The concentration of each ion in the steelmaking wastewater is Na + 700～900mg/L，K + 200～350mg/L，Ca 2+ 50～300mg/L，Zn 2+ 60～80mg/L，Cl - 1200～1600mg/L，SO 4 2- 150～300mg/L，NO 3 - 5～15mg/L，NH 4 + 400-900 mg/L; waste steel-makingThe pH value of the water is 8-13;
the converter flue gas contains 16-30% of CO and 16-30% of CO by volume 2 10～40％、N 2 36～46％、NO x 0～2％；
CO in the converter flue gas 2 The trapping rate of the catalyst is 90-99%.
2. The method for capturing carbon dioxide and co-producing NPCC in converter flue gas by closed cycle of converter steel slag and steelmaking wastewater according to claim 1, wherein the carbonization rate of calcium in the leaching solution is 95-100%.
3. The method for capturing carbon dioxide and co-producing NPCC in converter flue gas by closed cycle of converter steel slag and steelmaking wastewater as claimed in claim 1, wherein in step (3), the ratio of total volume of the introduced converter flue gas to total mass of the converter steel slag is 270-2390 m 3 /t。
4. The method for capturing carbon dioxide and co-producing NPCC in converter flue gas by closed cycle of converter steel slag-steelmaking wastewater according to claim 1, wherein in step (2), the desalination rate of calcium ions in the obtained liquid phase is 90-99%, and the pH value of the liquid phase is 6.2-7.2.
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| CN113443628A (en) * | 2021-06-18 | 2021-09-28 | 华中农业大学 | Carbon-neutralized solid waste leaching-CO2Mineralization circulation system and process |
| CN113750769A (en) * | 2021-11-10 | 2021-12-07 | 天津市新天钢钢铁集团有限公司 | Purification of sintering flue gas and solidification of CO by using LF refining waste residue2Method (2) |
| CN114684839B (en) * | 2022-03-07 | 2024-03-22 | 南京工程学院 | Hierarchical mineralization carbon fixation and product cascade utilization method for industrial byproduct gypsum |
| CN114849445A (en) * | 2022-03-22 | 2022-08-05 | 孙刚 | Method for cooperating pretreatment of industrial solid waste and carbon capture of flue gas |
| CN116462217B (en) * | 2023-01-18 | 2024-09-10 | 国家能源集团科学技术研究院有限公司 | Method for preparing calcium carbonate by utilizing steel slag |
| CN117185334A (en) * | 2023-09-22 | 2023-12-08 | 扬州一川镍业有限公司 | Method for preparing nano calcium carbonate by carbon dioxide adsorption through steel slag |
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