CN109821412B - Composite modified activated carbon for flue gas desulfurization and denitrification and preparation method thereof - Google Patents
Composite modified activated carbon for flue gas desulfurization and denitrification and preparation method thereof Download PDFInfo
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Abstract
The invention discloses composite modified activated carbon for flue gas desulfurization and denitrification and a preparation method thereof, and belongs to the field of solid waste resource utilization. The composite modified activated carbon comprises a composite modifier, a composite grinding aid, hydrochloric acid, activated carbon, absolute ethyl alcohol and water. The invention solves the problems that the conversion efficiency of the activated carbon to sulfide and nitrogen oxide is improved by utilizing the activated carbon to load metal active sites for modification in the prior art, so that the production and inactivation post-treatment costs of the activated carbon are higher; the activated carbon has low mechanical strength, easy pulverization and low ignition point; the coal gangue is hard to grind due to high hardness, the production cost of the modified activated carbon is reduced by 20-30%, and the market competitiveness and the application range of the modified activated carbon are improved. The active carbon is modified by the mixture of the red mud and the coal gangue in the sintering process to prepare the composite modified active carbon with superior flue gas desulfurization and denitrification performance and low cost, the high added value application of the red mud and the coal gangue in the sintering process is expanded, and a new idea of treating waste by waste is realized.
Description
Technical Field
The invention belongs to the field of solid waste resource utilization, and particularly relates to composite modified activated carbon for modifying activated carbon by using composite micro powder of sintering red mud and coal gangue and used for flue gas desulfurization and denitrification and a preparation method thereof.
Background
The steel industry is not only a supporting industry of national economic construction, but also a high-pollution industry with great influence on the environment. SO in the iron and steel industry2The emission and the emission of nitrogen oxides respectively account for 9.3 to 5.6 percent of the national emission, wherein the sintering process is mainly SO2And nitrogen oxide emission. In recent years, with the pollution (such as SO) of our country2Nitrogen oxides, etc.) to design and develop or introduce advanced pollutant control technology for sintering flue gas purification, for example, the flue gas desulfurization and denitration process of a thermal power plant is used for sintering flue gas purification of the iron and steel enterprises, but the ideal effect is obtained due to the emission characteristics of the sintering flue gas of the iron and steel enterprises. Thus, it is possible to provideResearch and development of a combined desulfurization and denitrification integrated process suitable for emission characteristics of sintering flue gas has become a focus of attention of iron and steel enterprises, wherein desulfurization and denitrification of sintering flue gas by using activated carbon are successfully applied to large-scale iron and steel companies in China, but the activated carbon used in the operation process has high operation cost, low mechanical strength, easy pulverization and low ignition point, has a risk of burning a tower, and has an SO adsorption effect on nitrogen oxides2The popularization of the activated carbon dry-method flue gas purification technology in the sintering flue gas purification technology of the iron and steel enterprises is greatly limited due to the existence of the problems.
The modification by using the active carbon loaded metal active site is an effective means for improving the conversion efficiency of the active carbon to sulfide and nitrogen oxide, but the active carbon loaded metal is mostly metal oxide, so that the production and inactivation post-treatment costs of the active carbon are higher. The red mud produced by sintering process is waste residue produced in the production process of alumina, and its main component is SiO2、CaO、Fe2O3、Al2O3、Na2O、TiO2MgO, etc. and also contains causticizing alkali component and trace nonferrous metal, in which CaO (37.2% -51.8%) and Al are contained2O3(4.5% -8.5%) and Fe2O3(7.8% -14.4%) higher content; the coal gangue is solid waste discharged in the coal mining process and the coal washing process, is a black gray rock which has lower carbon content and is harder than coal and is associated with a coal bed in the coal forming process, and the main component of the coal gangue is Al2O3、SiO2、Fe2O3、CaO、MgO、Na2O、K2O、P2O5、SO3And trace rare elements (gallium, vanadium, titanium, cobalt), wherein Al2O3(16.4％～36.7％)、SiO2(52.1％～65.5％)、Fe2O3(2.8% -14.6%) is higher. If alkaline substances and metal oxides contained in the red mud and the coal gangue in the sintering process are utilized to modify the activated carbon, the cost problem of the modified activated carbon for flue gas desulfurization and denitration is solved, the high-added-value application of the red mud and the coal gangue in the sintering process is expanded, and a new idea of treating waste with waste is realized.
Disclosure of Invention
The method aims to solve the problems that the conversion efficiency of the activated carbon to sulfide and nitrogen oxide is improved by utilizing the activated carbon to load metal active sites, so that the production cost and the treatment cost after inactivation of the activated carbon are higher; the activated carbon has low mechanical strength, easy pulverization and low ignition point; the coal gangue has high hardness, so the coal gangue is difficult to grind. According to the invention, the activated carbon is modified by using the composite micro powder of the red mud and the coal gangue in the sintering method to obtain the composite modified activated carbon, and the grinding speed, the grinding time, the ultrasonic power, the ultrasonic dispersion time, the drying temperature, the calcining temperature, the roasting time and the like are controlled, so that the high-added-value cyclic utilization of the red mud and the coal gangue in the sintering method is realized, and the composite modified activated carbon with excellent flue gas desulfurization and denitrification performance and low cost is obtained.
In order to solve the above technical problems, the present invention is realized by the following technical solutions.
The invention provides composite modified activated carbon for flue gas desulfurization and denitrification, which comprises the following raw materials in percentage by weight:
the composite modifier is a mixture of sintering process red mud and coal gangue, and the mass ratio of the sintering process red mud to the coal gangue is 1: 2-2: 1; the composite grinding aid is a mixture of ethylene glycol and absolute ethyl alcohol, the mass ratio of the ethylene glycol to the absolute ethyl alcohol is 1: 2-2: 1, and the ethylene glycol and the absolute ethyl alcohol are analytically pure; the hydrochloric acid is analytically pure; the active carbon is industrial pure; the absolute ethyl alcohol is analytically pure; the water is deionized water.
The invention also provides a preparation method of the composite modified activated carbon for flue gas desulfurization and denitration, which comprises the following steps:
firstly, mixing a composite modifier with a composite grinding aid, and then grinding for 90-120 min by using a variable frequency planetary ball mill at a rotating speed of 600-800 r/min to obtain composite modified micro powder.
And secondly, mixing the composite modified micro powder with water, ultrasonically dispersing for 30-60 min by using an ultrasonic cell disruptor with the ultrasonic power of 400-600W, sequentially adding hydrochloric acid, activated carbon and absolute ethyl alcohol, and ultrasonically dispersing for 60-90 min by using the ultrasonic cell disruptor with the ultrasonic power of 600-800W to obtain a composite modified activated carbon precursor.
And finally, placing the composite modified activated carbon precursor into a blast drying oven with the drying temperature of 70-90 ℃ for drying, and roasting for 15-30 min by using an experimental furnace with the calcining temperature of 200-300 ℃ to obtain the composite modified activated carbon.
The scientific principle of the invention is as follows:
(1) the surface active agent molecules of the composite grinding aid are utilized to form a monomolecular adsorption film on the surface of the mixture of the red mud and the coal gangue in the sintering process to be ground, the mixture of the red mud and the coal gangue in the sintering process is broken in the grinding process, and free electrovalence bonds generated on the broken surface of the mixture are neutralized with ions or molecules provided by the composite modifier, so that the aggregation tendency of the steel slag micropowder is eliminated or weakened, and the recombination of the broken surface is prevented.
(2) The composite grinding aid is adsorbed on the surface of the mixture of the red mud and the coal gangue in the sintering process, the composite grinding aid is utilized to perform wetting action and adsorption action on the mixture of the red mud and the coal gangue in the sintering process, the surface free energy of the mixture of the red mud and the coal gangue in the sintering process is reduced, the inter-grain resultant force of the mixture of the red mud and the coal gangue in the sintering process is weakened, and the extrusion crack seam stress is generated, so that the effect of destroying the hardness of the mixture of the red mud and the coal.
(3) CaO and Al in red mud by sintering method2O3With Fe2O3The content of (A) is higher; al in gangue2O3、SiO2、Fe2The content of O3 is high. Utilizes CaO with high alkalinity and SO in sintering flue gas2Generation of CaO + SO2→CaSO3The reaction is favorable for improving the desulfurization efficiency(ii) a Using Fe with catalytic reduction properties2O3The catalyst and the active carbon have synergistic effect to perform catalytic reduction on NO in the sintering flue gas, so that the denitration efficiency is improved; using a refractory Al substance with high melting point2O3With MgO and P in coal gangue2O5Produces synergistic flame-retardant effect and improves ignition point.
(4) The composite modified activated carbon utilizes the high adsorption performance of the activated carbon, the mixture of the sintering process red mud and the coal gangue has an alkaline absorption effect and a catalytic reduction effect on sulfides and nitrogen oxides in the flue gas, and the mixture of the sintering process red mud and the coal gangue has a synergistic flame retardant effect, so that the flue gas desulfurization and denitration performance and the ignition point of the composite modified activated carbon are improved.
Compared with the prior art, the invention has the following beneficial effects:
1. the invention solves the problems that the conversion efficiency of the activated carbon to sulfide and nitrogen oxide is improved by utilizing the activated carbon to load metal active sites for modification in the prior art, so that the production and inactivation post-treatment costs of the activated carbon are higher; the activated carbon has low mechanical strength, easy pulverization and low ignition point; the coal gangue is hard to grind due to high hardness, the production cost of the modified activated carbon is reduced by 20-30%, and the market competitiveness and the application range of the modified activated carbon are improved.
2. According to the invention, the activated carbon is modified by using the mixture of the red mud and the coal gangue in the sintering process to prepare the composite modified activated carbon with excellent flue gas desulfurization and denitrification performances and low cost, so that the high added value application of the red mud and the coal gangue in the sintering process is expanded, and a new idea of treating waste by waste is realized.
3. The composite modified activated carbon for flue gas desulfurization and denitrification and the preparation method thereof meet the policy requirements of relevant energy conservation, environmental protection and circular economy.
Detailed Description
The present invention will be described in detail with reference to specific examples, but the present invention is not limited to the examples.
Example 1
The components used for preparing 100g of the product of the invention and the mass ratio thereof are as follows:
the composite modifier is a mixture of sintering process red mud and coal gangue, and the mass ratio of the sintering process red mud to the coal gangue is 1: 1; the composite grinding aid is a mixture of ethylene glycol and absolute ethyl alcohol, the mass ratio of the ethylene glycol to the absolute ethyl alcohol is 1: 2, and the ethylene glycol and the absolute ethyl alcohol are analytically pure; the hydrochloric acid is analytically pure; the active carbon is industrial pure; the absolute ethyl alcohol is analytically pure; the water is deionized water.
Firstly, mixing a composite modifier with a composite grinding aid, and then grinding for 100min at a rotating speed of 800r/min by using a variable frequency planetary ball mill to obtain composite modified micro powder.
And secondly, mixing the composite modified micro powder with water, performing ultrasonic dispersion for 30min by using an ultrasonic cell disruptor with the ultrasonic power of 600W, sequentially adding hydrochloric acid, activated carbon and absolute ethyl alcohol, and performing ultrasonic dispersion for 90min by using the ultrasonic cell disruptor with the ultrasonic power of 700W to obtain a composite modified activated carbon precursor.
And finally, placing the composite modified activated carbon precursor into a blast drying oven with the drying temperature of 70 ℃ for drying, and roasting for 30min by using an experimental furnace with the calcining temperature of 250 ℃ to obtain the composite modified activated carbon.
Example 2
The components used for preparing 100g of the product of the invention and the mass ratio thereof are as follows:
the composite modifier is a mixture of sintering process red mud and coal gangue, and the mass ratio of the sintering process red mud to the coal gangue is 2: 1; the composite grinding aid is a mixture of glycol and absolute ethyl alcohol, the mass ratio of the glycol to the absolute ethyl alcohol is 1: 1, and the glycol and the absolute ethyl alcohol are analytically pure; the hydrochloric acid is analytically pure; the active carbon is industrial pure; the absolute ethyl alcohol is analytically pure; the water is deionized water.
Firstly, mixing a composite modifier with a composite grinding aid, and then grinding for 110min at a rotating speed of 600r/min by using a variable frequency planetary ball mill to obtain composite modified micro powder.
And secondly, mixing the composite modified micro powder with water, performing ultrasonic dispersion for 50min by using an ultrasonic cell disruptor with the ultrasonic power of 500W, sequentially adding hydrochloric acid, activated carbon and absolute ethyl alcohol, and performing ultrasonic dispersion for 70min by using an ultrasonic cell disruptor with the ultrasonic power of 800W to obtain a composite modified activated carbon precursor.
And finally, placing the composite modified activated carbon precursor into a blast drying oven with the drying temperature of 80 ℃ for drying, and roasting for 15min by using an experimental furnace with the calcining temperature of 300 ℃ to obtain the composite modified activated carbon.
Example 3
The components used for preparing 100g of the product of the invention and the mass ratio thereof are as follows:
the composite modifier is a mixture of sintering process red mud and coal gangue, and the mass ratio of the sintering process red mud to the coal gangue is 1: 2; the composite grinding aid is a mixture of glycol and absolute ethyl alcohol, the mass ratio of the glycol to the absolute ethyl alcohol is 2: 1, and the glycol and the absolute ethyl alcohol are analytically pure; the hydrochloric acid is analytically pure; the active carbon is industrial pure; the absolute ethyl alcohol is analytically pure; the water is deionized water.
Firstly, mixing a composite modifier with a composite grinding aid, and then grinding for 120min at a rotating speed of 700r/min by using a variable frequency planetary ball mill to obtain composite modified micro powder.
And secondly, mixing the composite modified micro powder with water, performing ultrasonic dispersion for 60min by using an ultrasonic cell disruptor with the ultrasonic power of 400W, sequentially adding hydrochloric acid, activated carbon and absolute ethyl alcohol, and performing ultrasonic dispersion for 60min by using an ultrasonic cell disruptor with the ultrasonic power of 600W to obtain a composite modified activated carbon precursor.
And finally, placing the composite modified activated carbon precursor into a blast drying oven with the drying temperature of 90 ℃ for drying, and roasting for 25min by using an experimental furnace with the calcining temperature of 200 ℃ to obtain the composite modified activated carbon.
Example 4
The components used for preparing 100g of the product of the invention and the mass ratio thereof are as follows:
the composite modifier is a mixture of sintering process red mud and coal gangue, and the mass ratio of the sintering process red mud to the coal gangue is 1: 2; the composite grinding aid is a mixture of glycol and absolute ethyl alcohol, the mass ratio of the glycol to the absolute ethyl alcohol is 1: 1, and the glycol and the absolute ethyl alcohol are analytically pure; the hydrochloric acid is analytically pure; the active carbon is industrial pure; the absolute ethyl alcohol is analytically pure; the water is deionized water.
Firstly, mixing a composite modifier with a composite grinding aid, and then grinding for 90min at a rotating speed of 800r/min by using a variable frequency planetary ball mill to obtain composite modified micro powder.
And secondly, mixing the composite modified micro powder with water, performing ultrasonic dispersion for 40min by using an ultrasonic cell disruptor with the ultrasonic power of 500W, sequentially adding hydrochloric acid, activated carbon and absolute ethyl alcohol, and performing ultrasonic dispersion for 80min by using the ultrasonic cell disruptor with the ultrasonic power of 600W to obtain a composite modified activated carbon precursor.
And finally, placing the composite modified activated carbon precursor into a forced air drying oven with the drying temperature of 90 ℃ for drying, and roasting for 20min by using an experimental furnace with the calcining temperature of 300 ℃ to obtain the composite modified activated carbon.
Example 5
The components used for preparing 100g of the product of the invention and the mass ratio thereof are as follows:
the composite modifier is a mixture of sintering process red mud and coal gangue, and the mass ratio of the sintering process red mud to the coal gangue is 1: 1; the composite grinding aid is a mixture of glycol and absolute ethyl alcohol, the mass ratio of the glycol to the absolute ethyl alcohol is 2: 1, and the glycol and the absolute ethyl alcohol are analytically pure; the hydrochloric acid is analytically pure; the active carbon is industrial pure; the absolute ethyl alcohol is analytically pure; the water is deionized water.
Firstly, mixing a composite modifier with a composite grinding aid, and grinding for 110min at a rotating speed of 700r/min by using a variable frequency planetary ball mill to obtain composite modified micro powder.
And secondly, mixing the composite modified micro powder with water, performing ultrasonic dispersion for 60min by using an ultrasonic cell disruptor with the ultrasonic power of 600W, sequentially adding hydrochloric acid, activated carbon and absolute ethyl alcohol, and performing ultrasonic dispersion for 70min by using an ultrasonic cell disruptor with the ultrasonic power of 800W to obtain a composite modified activated carbon precursor.
And finally, placing the composite modified activated carbon precursor into a blast drying oven with the drying temperature of 70 ℃ for drying, and roasting for 25min by using an experimental furnace with the calcining temperature of 250 ℃ to obtain the composite modified activated carbon.
Example 6
The components used for preparing 100g of the product of the invention and the mass ratio thereof are as follows:
the composite modifier is a mixture of sintering process red mud and coal gangue, and the mass ratio of the sintering process red mud to the coal gangue is 2: 1; the composite grinding aid is a mixture of ethylene glycol and absolute ethyl alcohol, the mass ratio of the ethylene glycol to the absolute ethyl alcohol is 1: 2, and the ethylene glycol and the absolute ethyl alcohol are analytically pure; the hydrochloric acid is analytically pure; the active carbon is industrial pure; the absolute ethyl alcohol is analytically pure; the water is deionized water.
Firstly, mixing a composite modifier with a composite grinding aid, and then grinding for 120min at a rotating speed of 600r/min by using a variable frequency planetary ball mill to obtain composite modified micro powder.
And secondly, mixing the composite modified micro powder with water, performing ultrasonic dispersion for 50min by using an ultrasonic cell disruptor with the ultrasonic power of 400W, sequentially adding hydrochloric acid, activated carbon and absolute ethyl alcohol, and performing ultrasonic dispersion for 90min by using the ultrasonic cell disruptor with the ultrasonic power of 700W to obtain a composite modified activated carbon precursor.
And finally, placing the composite modified activated carbon precursor into a blast drying oven with the drying temperature of 80 ℃ for drying, and roasting for 30min by using an experimental furnace with the calcining temperature of 200 ℃ to obtain the composite modified activated carbon.
Comparative example 1
The components used for preparing 100g of the product of the invention and the mass ratio thereof are as follows:
the composite modifier is a mixture of sintering process red mud and coal gangue, and the mass ratio of the sintering process red mud to the coal gangue is 2: 1; the active carbon is industrial pure; the absolute ethyl alcohol is analytically pure; the water is deionized water.
Firstly, grinding the composite modifier for 120min at the rotating speed of 600r/min by using a variable frequency planetary ball mill to obtain composite modified micro powder.
And secondly, mixing the composite modified micro powder with water, performing ultrasonic dispersion for 50min by using an ultrasonic cell disruptor with the ultrasonic power of 400W, sequentially adding hydrochloric acid, activated carbon and absolute ethyl alcohol, and performing ultrasonic dispersion for 90min by using the ultrasonic cell disruptor with the ultrasonic power of 700W to obtain a composite modified activated carbon precursor.
And finally, placing the composite modified activated carbon precursor into a blast drying oven with the drying temperature of 80 ℃ for drying, and roasting for 30min by using an experimental furnace with the calcining temperature of 200 ℃ to obtain the composite modified activated carbon.
Comparative example 2
The components used for preparing 100g of the product of the invention and the mass ratio thereof are as follows:
the hydrochloric acid is analytically pure; the active carbon is industrial pure; the absolute ethyl alcohol is analytically pure; the water is deionized water.
Firstly, ultrasonically dispersing water for 50min by using an ultrasonic cell disruptor with ultrasonic power of 400W, sequentially adding hydrochloric acid, activated carbon and absolute ethyl alcohol, and ultrasonically dispersing for 90min by using the ultrasonic cell disruptor with ultrasonic power of 700W to obtain an activated carbon precursor.
And then, putting the activated carbon precursor into a forced air drying oven with the drying temperature of 80 ℃ for drying, and roasting for 30min by using an experimental furnace with the calcining temperature of 200 ℃ to obtain the activated carbon.
The performance test procedures of the preparation examples 1-6 and the comparative examples 1-2 are as follows:
the inner diameter phi of the quartz tube fixed bed reactor is 35mm, 6g of composite modified activated carbon is fixed in the middle of the reaction bed in the experimental process, and the programmable controller is utilized to control the reaction temperature. Experimental atmosphere using N2、NO、NH3、SO2And O2In a gas mixing cylinder according to [ N ]2]84.8%, [ NO%]0.05% and [ NH ]3]0.05% and [ SO ]2]0.10% and [ O2]After 15 percent of the mixture is uniformly mixed, the mixture enters a fixed bed reactor to simulate industrial sintering flue gas, wherein the total flow of inlet gas is 600mL/min, and the volume space velocity is 3600h-1The reaction temperature was 120 ℃ and the reaction time was 8 h. Simulating SO in industrial sintering flue gas and tail gas by using flue gas analyzer2And (4) testing the concentration and the NO concentration. According to the activated carbon ignition point testThe firing point of the composite modified activated carbon is tested by the method GB/T20450-2006.
TABLE 1 Properties of composite modified activated carbon
Claims (2)
1. The composite modified activated carbon for desulfurization and denitrification of flue gas is characterized by comprising the following raw materials in percentage by weight:
the composite modifier is a mixture of sintering process red mud and coal gangue, and the mass ratio of the sintering process red mud to the coal gangue is 1: 2-2: 1; the composite grinding aid is a mixture of ethylene glycol and absolute ethyl alcohol, the mass ratio of the ethylene glycol to the absolute ethyl alcohol is 1: 2-2: 1, and the ethylene glycol and the absolute ethyl alcohol are analytically pure; the hydrochloric acid is analytically pure; the active carbon is industrial pure; the absolute ethyl alcohol is analytically pure; the water is deionized water.
2. The preparation method of the composite modified activated carbon for flue gas desulfurization and denitration according to claim 1, characterized by comprising the following steps:
firstly, mixing a composite modifier with a composite grinding aid, and grinding for 90-120 min by using a variable frequency planetary ball mill at a rotating speed of 600-800 r/min to obtain composite modified micro powder;
secondly, mixing the composite modified micro powder with water, ultrasonically dispersing for 30-60 min by using an ultrasonic cell disruptor with the ultrasonic power of 400-600W, sequentially adding hydrochloric acid, activated carbon and absolute ethyl alcohol, and ultrasonically dispersing for 60-90 min by using the ultrasonic cell disruptor with the ultrasonic power of 600-800W to obtain a composite modified activated carbon precursor;
and finally, placing the composite modified activated carbon precursor into a blast drying oven with the drying temperature of 70-90 ℃ for drying, and roasting for 15-30 min by using an experimental furnace with the calcining temperature of 200-300 ℃ to obtain the composite modified activated carbon.
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| US3917795A (en) * | 1970-11-30 | 1975-11-04 | Black Sivalls & Bryson Inc | Method of treating coal refuse |
| DE4102557A1 (en) * | 1991-01-29 | 1992-07-30 | Inst Energetik Gmbh | Catalytic absorbent prodn. from mixed inorganic and organic waste - contg. catalytic heavy metal and carbon by pyrolysis and activation, used in waste gas purificn. |
| CN1555906A (en) * | 2003-12-31 | 2004-12-22 | 卢伟林 | Composite desulfur agent and its manufacturing method and application |
| CN102211807B (en) * | 2011-05-04 | 2012-10-10 | 南京工业大学 | High-density porous support for treating wastewater of biological fluidized bed and preparation method thereof |
| CN105854807A (en) * | 2014-10-27 | 2016-08-17 | 安徽理工大学 | Composite adsorbing material based on straw and preparation method thereof |
| CN107051413B (en) * | 2017-01-10 | 2019-11-19 | 中国科学院过程工程研究所 | A method of iron-absorbent charcoal composite material is prepared by red mud and coal/charcoal |
| CN106881019A (en) * | 2017-02-23 | 2017-06-23 | 中国矿业大学 | A kind of method that utilization red mud and activated carbon thermal activation prepare desulfurizing agent |
| CN107213787A (en) * | 2017-06-29 | 2017-09-29 | 山东庚辰环保新材料有限公司 | A kind of desulfurizing agent and preparation method thereof |
| CN107899596A (en) * | 2017-10-30 | 2018-04-13 | 昆明理工大学 | A kind of desulfurization denitrification agent and preparation method thereof |
| CN108479744A (en) * | 2018-04-28 | 2018-09-04 | 孙燕霞 | A kind of preparation method and applications of desulphurization catalyst |
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