CN111715196B - Method for preparing magnetic activated carbon NaX molecular sieve composite material by taking coal gasification fine slag as raw material - Google Patents
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Abstract
The invention belongs to the technical field of environmental protection, and relates to a method for preparing a magnetic activated carbon NaX molecular sieve composite material by taking coal gasification fine slag as a raw material.
Description
The technical field is as follows:
the invention belongs to the technical field of environmental protection, and particularly relates to a method for preparing a magnetic activated carbon NaX molecular sieve composite material by taking coal gasification fine slag as a raw material.
The background art comprises the following steps:
the coal gasification technology is one of clean coal core technologies and is the basis of coal chemical industry. Coal gasification slag which is a byproduct generated in the process of preparing synthesis gas by high-temperature gasification of coal in a gasification furnace mainly comprises unburned carbon, metal oxide, sulfide and other substances and belongs to solid waste. The method is characterized in that the slag is divided into fine slag and coarse slag due to different discharge modes, wherein the coarse slag is waste slag discharged from the bottom of the furnace, and the fine slag is waste slag carried by top airflow. With the rapid development of coal gasification technology in China, a large amount of coal gasification slag is generated, if the coal gasification slag is randomly stacked, a large amount of land is occupied, and heavy metals in the coal gasification slag can leak into soil to cause environmental pollution. The recycling of the gasified slag not only can effectively solve the problem, but also can change waste into valuable and obtain economic benefit.
NaX type molecular sieves and activated carbon are two different adsorbents. The NaX type molecular sieve is a microporous molecular sieve with a hydrophilic surface, has regularly arranged molecular level pores, can only adsorb molecules with certain size, has adsorption selectivity and cation exchange capacity, and is a good adsorbent for adsorbing metal ions and catalysts. The activated carbon has large specific surface area, developed pores and hydrophilic surface, and is more suitable for the adsorption of organic matters. CN 201710154400.1 discloses a method for preparing an adsorption material by using coal gasification fine slag, which comprises sorting coal gasification fine slag to obtain a carbon-rich material, and activating with steam to obtain activated carbon, and CN 201710157486.3 discloses a method for preparing a carbon/silicon composite mesoporous material by using coal gasification coarse slag, wherein the coal gasification coarse slag is subjected to acid dissolution, alkali dissolution and activation to prepare the carbon/silicon composite mesoporous material. If the ferric oxide in the solution is treated to become ferromagnetic substance, the adsorption material can be recovered and recycled by utilizing the magnetic separation performance. Therefore, a novel method for preparing the magnetic activated carbon NaX molecular sieve composite material by taking the coal gasification fine slag as a raw material is urgently needed.
The invention content is as follows:
the invention aims to overcome the defects in the prior art, and provides a method for preparing a magnetic activated carbon NaX molecular sieve composite material by taking coal gasification fine slag as a raw material.
In order to realize the purpose, the specific process for preparing the magnetic activated carbon NaX molecular sieve composite material comprises the following steps:
(1) Pretreatment: drying the coal gasification fine slag at 105 ℃ until the quality is constant, then grinding and crushing the coal gasification fine slag by using a ball mill, and sieving the coal gasification fine slag with a 200-mesh sieve to obtain pretreated coal gasification fine slag;
(2) Melting, activating and reducing magnetizing treatment: and (3) mixing the solid alkali and the pretreated coal gasification fine slag according to the proportion of 1: 1-1: 3, putting the mixture into a tubular furnace after uniformly mixing, introducing argon gas with the flow rate of 200ml/min into the tubular furnace, heating the mixture to 600 ℃, then introducing steam, heating the mixture to 700-900 ℃, reacting for 1-3 hours, activating carbon components and steam in the coal gasification fine slag to obtain a mixed product, carrying out melting reaction on silicon-aluminum components and solid alkali in the coal gasification fine slag, and reducing ferric oxide into magnetic substance iron by reducing gases, namely hydrogen and carbon monoxide generated by the reaction of the steam and the carbon; wherein the flow rate of the water vapor is 0.5-1.5 ml/(min g);
(3) Preparation of a guiding agent solution: weighing 7.6g NaOH, 2.7g Al (OH) 3 Dissolving in 60mL water, heating and stirring for 3h, and adding 10g NaSiO 3 ·9H 2 Slowly adding O into the solution, and stirring for 1h at normal temperature to prepare an amorphous seed crystal guiding agent;
(4) Aging: fully mixing the mixed product obtained in the step (2), deionized water and 1-3 ml of directing agent solution, stirring at room temperature for 1-2 h, and standing for 12h to obtain a mixed solution, wherein the ratio of the deionized water to the mixed product, namely ml: g, is 3;
(5) Crystallization: and (5) transferring the mixed solution obtained in the step (4) into a stainless steel reaction kettle with a polytetrafluoroethylene lining, crystallizing at the temperature of 90-120 ℃ for 10-12 h, filtering and washing a solid product to be neutral, and drying in an oven at the temperature of 100 ℃ to obtain the magnetic activated carbon NaX molecular sieve composite material.
The coal gasification fine slag is the residue which is carried by coal gasification gas and is separated and discharged in the purification process after the coal gasification gas leaves the coal gasification furnace.
The solid alkali is one or a mixture of two of sodium carbonate and sodium hydroxide.
Compared with the prior art, the magnetic activated carbon NaX molecular sieve composite material is prepared by taking the coal gasification fine slag as a raw material, the components of the coal gasification fine slag are utilized to the maximum extent, the carbon components in the coal gasification fine slag are activated into activated carbon, the silicon-aluminum component is hydrothermally crystallized into the molecular sieve, and ferric oxide is reduced into iron.
Description of the drawings:
fig. 1 is a graph of the X-ray diffraction analysis result of the magnetic activated carbon NaX molecular sieve composite material prepared in example 1 of the present invention, wherein Theta is the diffraction angle, and Intensity is the diffraction Intensity.
Fig. 2 is a graph of the result of measuring the saturation magnetization of the magnetic activated carbon NaX molecular sieve composite material prepared in example 1 of the present invention, where He is coercive force and Ms is saturation magnetization.
The specific implementation mode is as follows:
the invention is further illustrated by the following examples in conjunction with the accompanying drawings.
Example 1:
the specific process for preparing the magnetic activated carbon NaX molecular sieve composite material in the embodiment is as follows:
(1) Pretreatment: drying the coal gasification fine slag at 105 ℃ until the quality is constant, then grinding and crushing the coal gasification fine slag by using a ball mill, and sieving the coal gasification fine slag with a 200-mesh sieve to obtain pretreated coal gasification fine slag;
(2) Melting, activating and reducing magnetic endowing treatment: and (3) mixing the solid alkali and the pretreated coal gasification fine slag according to the proportion of 1:2, putting the mixture into a tubular furnace, introducing argon gas with the flow rate of 200ml/min, heating the mixture to 600 ℃, introducing steam with the flow rate of 0.5 ml/(min g), heating the mixture to 700 ℃, reacting for 1 hour, activating carbon components and steam in the gasified fine slag to obtain a mixed product, carrying out melting reaction on silicon-aluminum components in the gasified fine slag and solid alkali, and reducing ferric oxide in the gasified fine slag into magnetic substance iron by reducing gas hydrogen and carbon monoxide generated by the reaction of the steam and the carbon;
(3) Preparation of a guiding agent solution: weighing 7.6g NaOH, 2.7g Al (OH) 3 Dissolving in 60mL water, addingStirred hot for 3h, then 10g NaSiO 3 ·9H 2 Slowly adding O into the solution, and stirring for 1h at normal temperature to prepare an amorphous crystal seed guiding agent;
(4) Aging: fully mixing the mixed product obtained in the step (2), a certain amount of deionized water and 1ml of guiding agent solution, stirring for 2h at room temperature, and then standing for 12h, wherein the ratio ml of deionized water to mixed product is (g) is 3;
(5) And (3) crystallization: and transferring the mixed solution into a stainless steel reaction kettle with a polytetrafluoroethylene lining, crystallizing at the temperature of 120 ℃ for 12 hours, filtering and washing the solid product to be neutral, and drying in an oven at the temperature of 100 ℃ to obtain the magnetic activated carbon NaX molecular sieve composite material.
Example 2:
the specific process for preparing the magnetic activated carbon NaX molecular sieve composite material in the embodiment is as follows:
(1) Pretreatment: drying the coal gasification fine slag at 105 ℃ until the quality is constant, and then grinding and crushing the coal gasification fine slag by using a ball mill to ensure that the particle size of the coal gasification fine slag is 200 meshes;
(2) Melting, activating and reducing magnetizing treatment: mixing solid alkali and coal gasification fine slag according to the proportion of 1:1, putting the mixture into a tubular furnace, introducing 200ml/min argon at the same time, pouring the mixture into water vapor at the same time of 600 ℃ at the same time of heating, introducing 1 ml/(min g) water vapor at the same time of heating to 900 ℃, reacting for 3h, activating carbon components and water vapor in the gasified fine slag to obtain a mixed product, carrying out melting reaction on silicon-aluminum components in the gasified fine slag and solid alkali, and reducing ferric oxide in the gasified fine slag into magnetic substance iron by reducing gas hydrogen and carbon monoxide generated by the reaction of the water vapor and the carbon;
(3) Preparation of a guiding agent solution: weighing 7.6g NaOH, 2.7g Al (OH) 3 Dissolved in 60mL of water, heated and stirred for 3 hours, and then 10g of NaSiO 3 ·9H 2 Slowly adding O into the solution, and stirring for 1h at normal temperature to prepare an amorphous seed crystal guiding agent;
(4) Aging: fully mixing the mixed product obtained in the step (2), a certain amount of deionized water and 3ml of guiding agent solution, stirring for 2h at room temperature, and then standing for 12h, wherein the ratio ml of deionized water to mixed product is (g is 6);
(5) Crystallization: and transferring the mixed solution into a stainless steel reaction kettle with a polytetrafluoroethylene lining, crystallizing at the temperature of 120 ℃ for 10 times, filtering and washing a solid product to be neutral, and drying in an oven at the temperature of 100 ℃ to obtain the magnetic activated carbon NaX molecular sieve composite material.
Example 3:
the preparation method of the magnetic activated carbon NaX molecular sieve composite material comprises the following steps:
(1) Pretreatment: drying the coal gasification fine slag at 105 ℃ until the quality is constant, and then grinding and crushing the coal gasification fine slag by using a ball mill to ensure that the grain diameter of the coal gasification fine slag is 200 meshes;
(2) Melting, activating and reducing magnetic endowing treatment: mixing solid alkali and coal gasification fine slag according to the proportion of 1:3, putting the mixture into a tubular furnace, introducing argon gas with the flow rate of 200ml/min, heating the mixture to 600 ℃, then introducing steam with the flow rate of 1.5 ml/(min g), heating the mixture to 850 ℃, and reacting for 2 hours to activate carbon components and steam in the gasified fine slag to obtain a mixed product, wherein silicon-aluminum components in the gasified fine slag and solid alkali are subjected to melting reaction, and ferric oxide in the gasified fine slag is reduced into magnetic substance iron by reducing gas hydrogen and carbon monoxide generated by the reaction of the steam and the carbon;
(3) Preparation of a guiding agent solution: weighing 7.6g NaOH, 2.7g Al (OH) 3 Dissolved in 60mL of water, heated and stirred for 3 hours, then 10g of NaSiO 3 ·9H 2 Slowly adding O into the solution, and stirring for 1h at normal temperature to prepare an amorphous seed crystal guiding agent;
(4) Aging: fully mixing the obtained mixed product obtained in the step (2), a certain amount of deionized water and 2ml of guiding agent solution, stirring at room temperature for 2h, and then standing for 12h, wherein the liquid-solid ratio ml of the deionized water to the mixed product is 5;
(5) And (3) crystallization: and transferring the mixed solution into a stainless steel reaction kettle with a polytetrafluoroethylene lining, crystallizing at the temperature of 120 ℃ for 12 hours, filtering and washing the solid product to be neutral, and drying in an oven at the temperature of 100 ℃ to obtain the magnetic activated carbon NaX molecular sieve composite material.
Example 4:
in this example, the surface area of the magnetic activated carbon NaX molecular sieve composite material prepared in example 1 was measured by a specific surface area analyzer model ASAP2020, which is a company of mack instruments, and the specific surface area was measured to be 400.66m 2 (ii)/g, X-ray diffraction analysis was carried out using an X-ray diffractometer model Japanese Rigaku D/max 2500PC, the results of which are shown in FIG. 1; the saturation magnetization of the sample was measured by a SQUID-VSM type vibration sample magnetometer manufactured by Quantum Design, usa, and the result is shown in fig. 2; as can be seen from figure 1, the crystal phase structure of the product is a typical FAU structure and belongs to a NaX type molecular sieve, the saturation magnetization is 39.16emu/g as can be seen from figure 2, in order to further verify the recovery effect of the composite material, 2g of the product in example 1 is taken and placed in a container filled with deionized water, then the product is recovered by a magnet, the yield is 1.70g after drying and weighing, and the recovery rate reaches 85 percent, so that the magnetic activated carbon NaX molecular sieve composite material prepared by the method can be subjected to magnetic separation, and the recovery rate is high.
This example carried out Cu adsorption on the magnetic activated carbon NaX molecular sieve composite prepared in examples 1-3 2+ Respectively detecting the adsorption performance of the Cu-containing catalyst in the wastewater removal 2+ In the experiment, 100mg of the magnetic activated carbon NaX molecular sieve composite material is placed in a volume of 500ml and a Cu-containing molecular sieve composite material with a concentration of 100mg/L at a temperature of 25 DEG C 2+ The adsorption time in the wastewater is 3h, the experiments are repeated for three times, the average value is taken, the adsorption results are listed in table 1, and the adsorption results in table 1 show that the magnetic activated carbon NaX molecular sieve composite material prepared by the preparation method can be used for treating Cu in the wastewater 2+ The adsorption rate of the adsorbent is up to more than 99%, and the adsorbent has good adsorption performance.
Table 1: cu 2+ Results before and after treatment of overproof waste water
Claims (3)
1. A method for preparing a magnetic activated carbon NaX molecular sieve composite material by taking coal gasification fine slag as a raw material is characterized by comprising the following specific steps:
(1) Pretreatment: drying the coal gasification fine slag at 105 ℃ until the quality is constant, then grinding and crushing the coal gasification fine slag by using a ball mill, and sieving the coal gasification fine slag with a 200-mesh sieve to obtain pretreated coal gasification fine slag;
(2) Melting, activating and reducing magnetizing treatment: and (3) mixing the solid alkali and the pretreated coal gasification fine slag according to the proportion of 1:2, uniformly mixing, putting the mixture into a tubular furnace, introducing argon gas with the flow of 200mL/min and the like until the temperature is raised to 600 ℃, then introducing steam with the flow of 0.5 mL/(min g), raising the temperature to 700 ℃, and reacting for 1 hour, activating carbon components and steam in the gasified fine slag to obtain a mixed product, carrying out melting reaction on silicon-aluminum components and solid alkali in the gasified fine slag, and reducing ferric oxide in the gasified fine slag into magnetic substance iron by reducing gas hydrogen and carbon monoxide generated by the reaction of the steam and the carbon;
(3) Preparation of a guiding agent solution: weighing 7.6g NaOH, 2.7g Al (OH) 3 Dissolved in 60mL of water, heated and stirred for 3 hours, then 10g of NaSiO 3 ·9H 2 Slowly adding O into the solution, and stirring for 1h at normal temperature to prepare an amorphous seed crystal guiding agent;
(4) Aging: fully mixing the mixed product obtained in the step (2), a certain amount of deionized water and 1mL of guiding agent solution, stirring at room temperature for 2h, and then standing for 12h, wherein the liquid-solid ratio mL: g of the deionized water to the mixed product is 3;
(5) And (3) crystallization: transferring the mixed solution into a stainless steel reaction kettle with a polytetrafluoroethylene lining, crystallizing at the temperature of 120 ℃ for 12 hours, filtering and washing a solid product to be neutral, and drying in an oven at the temperature of 100 ℃ to obtain the magnetic activated carbon NaX molecular sieve composite material, wherein the specific surface area of the composite material is 400.66m 2 (ii)/g, saturation magnetization of 39.16emu/g, for Cu in sewage 2 + The adsorption rate of (2) was 99.4%.
2. The method for preparing the magnetic activated carbon NaX molecular sieve composite material by using the coal gasification fine slag as the raw material according to claim 1, characterized in that the coal gasification fine slag is a residue which is carried by coal gasification gas and is discharged in the purification process after the coal gasification gas leaves a coal gasification furnace.
3. The method for preparing the magnetic activated carbon NaX molecular sieve composite material by using the coal gasification fine slag as the raw material according to claim 1, wherein the solid alkali is one or a mixture of two of sodium carbonate and sodium hydroxide.
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| CN112830501B (en) * | 2021-01-21 | 2023-12-01 | 西安建筑科技大学华清学院 | Gasifier slag-based geopolymer molecular sieve, preparation method and application |
| CN113333436B (en) * | 2021-05-21 | 2022-04-08 | 中国矿业大学 | All-component comprehensive utilization method of coal gasification fine slag |
| CN114904484A (en) * | 2022-05-10 | 2022-08-16 | 宁波诺丁汉大学 | Method for preparing carbon-silicon composite material by using coal gasifier coarse slag |
| CN114906847A (en) * | 2022-05-16 | 2022-08-16 | 内蒙古科技大学 | Wet activation method for gasification slag carbon residue and application thereof |
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