CN110327874B - Core-shell structure composite iron-cerium oxide dearsenic adsorbent and preparation method and application thereof - Google Patents
Core-shell structure composite iron-cerium oxide dearsenic adsorbent and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a core-shell structure composite ferro-cerium oxide dearsenic adsorbent, which is magnetic nano Fe3O4As core, in the magnetic nano Fe3O4The surface is coated with a composite iron cerium oxide layer; the molar ratio of the iron element to the cerium element in the iron-cerium oxide layer is 1 (0.04-0.12). The preparation method of the dearsenic adsorbent comprises the following steps: magnetic nano Fe3O4Adding m-phenylenediamine and formaldehyde into the solution to carry out in-situ polymerization reaction to obtain a sample A; carbonizing the sample A at high temperature to obtain a sample B; loading the mixed solution of ferric nitrate and cerium nitrate on the sample B by an impregnation method to obtain a sample C; and oxidizing and roasting the sample C to obtain the de-arsenic adsorbent. The core-shell structure composite iron-cerium oxide dearsenifying adsorbent can directly capture gaseous arsenic in a larger temperature range, the arsenic adsorption efficiency can reach more than 80%, the arsenic is high in stability after adsorption, and secondary pollution of the arsenic is reduced.
Description
Technical Field
The invention belongs to the field of adsorbents, and particularly relates to an adsorbent suitable for treating arsenic-containing flue gas generated in a pyrometallurgical smelting process of nonferrous metal smelting.
Background
Because arsenic is extremely toxic, how to realize the efficient control of arsenic pollution emission becomes an urgent problem to be solved. Arsenic is definitely listed as a main prevention and control object in a series of documents such as national arsenic pollution prevention and control technical policy, comprehensive heavy metal pollution prevention and control planning (2011-2015), and thirteen-five ecological environment protection planning, which are issued in China, and the prevention and control of arsenic pollution becomes a focus of attention at home and abroad and a significant civil problem in China. In the process of smelting metal minerals, most of arsenic element in the ore is oxidized and volatilized into flue gas in the form of arsenic trioxide, and further arsenic-containing flue gas is formed.
At present, arsenic in smelting flue gas is mainly removed in the processes of dust removal and wet scrubbing, and the arsenic is transferred from the flue gas into soot and contaminated acid, so that the arsenic pollution risk still exists, and therefore, the direct capture and selective separation of gaseous arsenic captured from the flue gas become the main research direction for controlling the arsenic pollution. Chinese patent 201711220671.9 discloses a method for preparing a flue gas de-arsenic adsorbent, which is prepared by uniformly mixing calcium oxide, metallurgical slag, zeolite and fly ash, granulating, heating and the like; chinese patent 201810285567.6 discloses an arsenic adsorbent, and its preparation method and application, wherein an alumina carrier is impregnated with iron element and calcined at high temperature to prepare gaseous arsenic adsorbent. Although the adsorbent can realize the adsorption of gaseous arsenic, the adsorbent after adsorbing arsenic is still mixed with smoke dust or contaminated acid, is difficult to separate controllably, and faces the problem of secondary pollution of arsenic. In addition, the traditional adsorption material has low adsorption capacity and adsorption rate to gaseous arsenic, and is difficult to meet the requirements of actual industry. There is therefore a need to develop a stable, efficient and easily recyclable adsorbent material.
Disclosure of Invention
The invention aims to solve the technical problems that the defects and shortcomings in the background technology are overcome, and the preparation method of the recyclable high-efficiency arsenic removal adsorbent and the application method of the adsorbent for capturing gaseous arsenic are provided, so that the method is suitable for efficiently capturing and separating the gaseous arsenic in the high-temperature high-sulfur smelting flue gas.
In order to solve the technical problems, the technical scheme provided by the invention is as follows:
a composite Fe-Ce oxide de-arsenic adsorbent with core-shell structure is prepared from magnetic nano Fe3O4As core, in the magnetic nano Fe3O4The surface is coated with a composite iron cerium oxide layer; the molar ratio of the iron element to the cerium element in the iron-cerium oxide layer is 1 (0.04-0.12).
The invention also provides a preparation method of the dearsenic adsorbent, which comprises the following steps:
(1) will be magneticRice Fe3O4Adding m-phenylenediamine and formaldehyde into the solution, uniformly mixing by ultrasonic, and carrying out in-situ polymerization reaction under mechanical stirring to obtain a sample A;
(2) carbonizing the sample A at high temperature to obtain a sample B wrapped by a porous carbon material;
(3) loading the mixed solution of ferric nitrate and cerium nitrate on the sample B by an impregnation method, and drying to obtain a sample C loaded with iron and cerium;
(4) and oxidizing and roasting the sample C in an oxidizing atmosphere to obtain the de-arsenic adsorbent.
In the above preparation method, preferably, in the step (1), the magnetic nano-Fe3O4Has a particle diameter of 50 to 200 nm.
In the above preparation method, preferably, in the step (1), the molar ratio of m-phenylenediamine to formaldehyde is 1: (1.5-3), the pH value of the mixed solution is 8-9, and the in-situ polymerization reaction time is 18-30 h.
In the preparation method, preferably, in the step (2), the roasting temperature of high-temperature carbonization is 600-700 ℃, and the heat preservation time is 1.5-3 hours; the high-temperature carbonization is carried out under the protection of nitrogen, and the flow rate of the nitrogen is 0.5-1L/min.
In the preparation method, preferably, in the step (3), the molar ratio of the iron ions to the cerium ions is 1 (0.04-0.12), and the volume ratio of the mixed solution of ferric nitrate and cerium nitrate to the sample B is 1: (1-1.5), the dipping temperature is 25-50 ℃, and the dipping time is 30-60 min.
In the preparation method, preferably, in the step (4), the oxidizing roasting temperature is 600-800 ℃, the roasting time is 20-40 min, and the oxygen concentration is 20-40%.
As a general inventive concept, the invention also provides an application of the arsenic removal adsorbent or the arsenic removal adsorbent prepared by the preparation method in high-temperature and high-sulfur flue gas, the arsenic removal adsorbent is directly and uniformly sprayed into the flue gas at the front end of a flue gas dust collection process, the adsorbent adsorbing arsenic enters smoke dust together with the flue gas in a dust removal system to obtain arsenic-containing mixed smoke dust, and then the composite magnetic adsorbent is recovered from the arsenic-containing mixed smoke dust through magnetic separation.
In the application, preferably, the temperature of the flue gas is 400-1200 ℃ when the arsenic removal adsorbent is used for removing arsenic, and the concentration of sulfur dioxide in the flue gas is not higher than 10%.
The invention relates to a core-shell structure composite ferro-cerium oxide dearsenization adsorbent which is made of magnetic Fe3O4The particles are taken as the inner core and are polymerized in situ on the surface of Fe3O4Coating a layer of resin on the surface of the particles, forming a carbon shell with a loose and porous surface after high-temperature carbonization, forming various functional groups such as amino, carboxyl and the like in the high-temperature carbonization process, having certain adsorption capacity on metal ions, ensuring that the effective load of iron and cerium is realized by an impregnation method, finally oxidizing and roasting to oxidize and decompose the porous carbon layer, and converting the adsorbed iron and cerium into porous high-activity x (CeO)2)·y(Fe2O3) (wherein x/y is (0.08-0.24): 1) composite oxide, i.e. the final product is Fe3O4As an inner core and with a porous x (CeO)2)·y(Fe2O3) Composite adsorbing material with composite oxide As shell and gaseous As in flue gas2O3May be coated with CeO2Efficient oxidation to As2O5And is combined with Fe2O3Form stable ferric arsenate, thereby realizing the high-efficiency capture of gaseous arsenic. The small size and the physical characteristics of the composite adsorbent rich in pores ensure the adsorption rate of arsenic, the high-activity iron-cerium composite oxide ensures the efficient capture of arsenic, and the magnetic core of the composite adsorption material ensures the recoverability of the adsorbent.
Compared with the prior art, the invention has the advantages that:
(1) the core-shell structure composite iron-cerium oxide dearsenifying adsorbent can directly capture gaseous arsenic in a larger temperature range, the arsenic adsorption efficiency can reach more than 80%, the arsenic is high in stability after adsorption, and secondary pollution of the arsenic is reduced.
(2) The core-shell structure composite iron-cerium oxide dearsenifying adsorbent can be widely applied to the fields of smelting and coal-fired flue gas dearsenification, has a wide application range, can be directly applied to the existing flue gas treatment equipment, and does not need to change the existing treatment process.
(3) The core-shell structure composite iron-cerium oxide dearsenifying adsorbent can be recycled after desorption, so that the dearsenifying cost is reduced.
(4) The invention has the advantages of simple preparation process, high adsorption efficiency, environmental friendliness and the like.
Detailed Description
In order to facilitate an understanding of the invention, the invention will now be described more fully and in detail with reference to the preferred embodiments, but the scope of the invention is not limited to the specific embodiments described below.
Unless otherwise defined, all terms of art used hereinafter have the same meaning as commonly understood by one of ordinary skill in the art. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the scope of the present invention.
Unless otherwise specifically stated, various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or can be prepared by existing methods.
Example 1:
the preparation method of the core-shell structure composite iron cerium oxide dearsenic adsorbent comprises the following steps:
(1) 30mg of Fe with the grain diameter of 100nm is taken3O4Placing the particles into a solution containing 0.02mol of m-phenylenediamine and 0.04mol of formaldehyde, mixing the solution with ammonia water until the pH value is 8.5, reacting for 24 hours under continuous mechanical stirring, drying in a vacuum drying oven, placing in a tubular furnace, carbonizing at 650 ℃ for 3 hours under the protection of nitrogen gas to obtain porous carbon coated Fe3O4@ C adsorbent.
(2) Preparing 20mL of mixed solution with different molar ratios of iron and cerium, and mixing the mixed solution with the prepared Fe3O4Mixing @ C, impregnating Fe-Ce ions into Fe3O4Drying and removing water on @ C to finally obtain the composite adsorbents with different iron and cerium impregnation amounts;
(3) placing the composite adsorbent material in a tubular furnace, introducing gas with oxygen content of 30%, heating at a heating rate of 10 deg.C/minThe temperature is increased to 650 ℃, then the heat preservation time is 30min, and finally the Fe with different iron-cerium ratios and core-shell structures is obtained3O4@x(CeO2)·y(Fe2O3) An adsorbent.
Respectively taking 20mg of Fe with different iron-cerium ratios3O4@x(CeO2)·y(Fe2O3) And the adsorbent and the simulated arsenic-containing flue gas are sprayed into a quartz tube in the muffle furnace together, and filter cloth is arranged at the tail end of the quartz tube to collect the adsorbent. The conditions during the experiment were: the arsenic content in the simulated flue gas is 0.2mg, the flow rate of the flue gas is 0.1L/min, the temperature of the flue gas is 600 ℃, and the content of the gas in the flue gas is 20 percent of O2+5％SO2+55％N2The arsenic capture efficiency of the different adsorbents synthesized is shown in table 1.
TABLE 1 comparison of arsenic adsorption efficiency of composite adsorbents with different Fe/Ce ratios
Table 1 shows the comparison of arsenic capture efficiency of different fe-ce ratio composite adsorbents. It can be seen from the table that when the cerium content in the adsorbent is low (the iron-cerium ratio is 1: 0.02), the arsenic capture efficiency is only 30.6%, and a proper amount of cerium can promote the oxidation and adsorption of arsenic, so that the arsenic capture efficiency can be remarkably improved by increasing the cerium content. When the iron-cerium ratio is 1: at 0.16, the arsenic capture efficiency drops instead, indicating that the proper iron-cerium ratio plays a key role in the arsenic capture efficiency of the composite sorbent.
Example 2:
the preparation method of the core-shell structure composite iron cerium oxide dearsenic adsorbent comprises the following steps:
(1) 30mg of Fe with the grain diameter of 100nm is taken3O4Placing the particles into a solution containing 0.02mol of m-phenylenediamine and 0.04mol of formaldehyde, mixing the solution with ammonia water until the pH value is 8.5, reacting for 24 hours under continuous mechanical stirring, drying in a vacuum drying oven, placing in a tubular furnace, carbonizing at 650 ℃ for 3 hours under the protection of nitrogen gas to obtain porous carbon coated Fe3O4@ C adsorbent;
(2) preparing a mixture with the molar ratio of iron to cerium of 1: 20mL of 0.06 mixed solution and mixing it with prepared Fe3O4Mixing @ C, impregnating Fe-Ce ions into Fe3O4Drying and removing water on @ C to obtain a composite material;
(3) placing the composite material in a tubular furnace, introducing gas with the oxygen content of 30%, heating to 650 ℃ at the heating rate of 10 ℃/min, and then keeping the temperature for 30min to finally obtain the Fe with the core-shell structure3O4@0.12(CeO2)·(Fe2O3) An adsorbent. Taking 20mg of Fe3O4@0.12(CeO2)·(Fe2O3) An adsorbent.
Taking the Fe prepared in this example3O4@0.12(CeO2)·(Fe2O3) And 20mg, spraying the adsorbent and the simulated arsenic-containing flue gas into a quartz tube in a muffle furnace, and mounting filter cloth at the tail end of the quartz tube to collect the adsorbent. The conditions during the experiment were: simulating that the arsenic content in the flue gas is 0.2mg, the flow rate of the flue gas is 0.1L/min, the temperature of the flue gas is 600 ℃, and inspecting Fe under different conditions by changing the components and the reaction temperature of the flue gas3O4@0.12(CeO2)·(Fe2O3) The specific results of arsenic capture efficiency are shown in table 2.
TABLE 2 comparison of arsenic adsorption efficiency under different process conditions
Table 2 shows the comparison of the arsenic capturing performance under different atmospheres and capturing temperatures, and it can be seen from the table that the presence of oxygen and sulfur dioxide in the flue gas both promote the capturing of arsenic, while the presence of oxygen and sulfur dioxide in the actual smelting flue gas both promote the capturing of arsenic, so that the core-shell structure Fe3O4@0.12(CeO2)·(Fe2O3) The composite adsorbent is very suitable for capturing arsenic in smelting flue gas. The capture temperature is also an important parameter in practical application, the capture of arsenic is not facilitated when the temperature of the flue gas is lower or higher, the optimal capture temperature of arsenic is 600-800 ℃, and the capture efficiency of arsenic is over 80%. But the arsenic capture efficiency is still maintained above 60% at the reaction temperature of 400-1200 ℃, thus the method still has practical application value.
40mg of prepared Fe was taken3O4@0.12(CeO2)·(Fe2O3) The adsorbent and the simulated arsenic-containing flue gas are sprayed into a quartz tube arranged in a muffle furnace, and filter cloth is arranged at the tail end of the quartz tube to collect the adsorbent. The conditions during the experiment were: the arsenic content in the simulated flue gas is 0.2mg, the flow rate of the flue gas is 0.1L/min, the temperature of the flue gas is 600 ℃, the concentration of sulfur dioxide is 5%, and the concentration of oxygen is 20%. After the adsorption experiment, the adsorbent was regenerated by alkaline desorption and arsenic desorption and thermal activation, and the capture efficiency of the adsorbent for gas-phase arsenic was measured under the same conditions, and the cycle was repeated 5 times, and the specific results are shown in table 3. As can be seen from table 3, although the capture efficiency of the composite adsorbent for arsenic is somewhat reduced with the increase of the cycle number, the adsorption efficiency of the adsorbent for arsenic can be maintained at 64.23% after 5 cycles, which also indicates that the core-shell structure composite iron-cerium oxide adsorbent prepared by the present invention has excellent cycle performance.
TABLE 3 magnetic composite Fe3O4@0.12(CeO2)·(Fe2O3) Cycle performance of adsorbent
Claims (9)
1. The core-shell structure composite iron-cerium oxide dearsenic adsorbent applied to high-temperature high-sulfur flue gas is characterized in that the dearsenic adsorbent is magnetic nano Fe3O4As core, in the magnetic nano Fe3O4Surface coating with compoundA layer of iron cerium oxide; the molar ratio of the iron element to the cerium element in the iron-cerium oxide layer is 1 (0.08-0.12).
2. A method of preparing the de-arsenic adsorbent of claim 1, comprising the steps of:
(1) magnetic nano Fe3O4Adding m-phenylenediamine and formaldehyde into the solution, uniformly mixing by ultrasonic, and carrying out in-situ polymerization reaction under mechanical stirring to obtain a sample A;
(2) carbonizing the sample A at high temperature to obtain a sample B wrapped by a porous carbon material;
(3) loading the mixed solution of ferric nitrate and cerium nitrate on the sample B by an impregnation method, and drying to obtain a sample C loaded with iron and cerium;
(4) and oxidizing and roasting the sample C in an oxidizing atmosphere to obtain the dearsenic adsorbent.
3. The method according to claim 2, wherein in the step (1), the magnetic nano Fe3O4Has a particle diameter of 50 to 200 nm.
4. The method according to claim 2, wherein in the step (1), the molar ratio of m-phenylenediamine to formaldehyde is 1: (1.5-3), the pH value of the mixed solution is 8-9, and the in-situ polymerization reaction time is 18-30 h.
5. The preparation method according to claim 2, wherein in the step (2), the roasting temperature of the high-temperature carbonization is 600-700 ℃, and the holding time is 1.5-3 hours; the high-temperature carbonization is carried out under the protection of nitrogen, and the flow rate of the nitrogen is 0.5-1L/min.
6. The preparation method according to claim 2, wherein in the step (3), the molar ratio of the iron ions to the cerium ions is 1 (0.08-0.12), and the volume ratio of the mixed solution of the ferric nitrate and the cerium nitrate to the sample B is 1: (1-1.5); the dipping temperature in the dipping process is 25-50 ℃, and the dipping time is 30-60 min.
7. The preparation method according to claim 2, wherein in the step (4), the oxidizing roasting temperature is 600-800 ℃, the roasting time is 20-40 min, and the oxygen concentration is 20-40%.
8. The application of the arsenic-removing adsorbent according to claim 1 or the arsenic-removing adsorbent prepared by the preparation method according to any one of claims 2 to 7 in high-temperature and high-sulfur flue gas is characterized in that the arsenic-removing adsorbent is directly and uniformly sprayed into the flue gas at the front end of a flue gas dust collection process, the adsorbent adsorbing arsenic and the flue gas enter the flue gas in a dust removal system together to obtain arsenic-containing mixed flue gas, and then the composite magnetic adsorbent is recovered from the arsenic-containing mixed flue gas through magnetic separation.
9. The application of claim 8, wherein the temperature range of the flue gas when the arsenic removal adsorbent is used for removing arsenic is 400-1200 ℃, and the concentration of sulfur dioxide in the flue gas is not higher than 10%.
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