CN106669678B - Preparation method of catalyst for electrocatalytic degradation of organic wastewater - Google Patents
Preparation method of catalyst for electrocatalytic degradation of organic wastewater Download PDFInfo
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- 239000003054 catalyst Substances 0.000 title claims abstract description 47
- 239000002351 wastewater Substances 0.000 title abstract description 17
- 238000002360 preparation method Methods 0.000 title abstract description 15
- 230000015556 catabolic process Effects 0.000 title abstract description 10
- 238000006731 degradation reaction Methods 0.000 title abstract description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 78
- 238000000034 method Methods 0.000 claims abstract description 39
- 239000007795 chemical reaction product Substances 0.000 claims abstract description 36
- 239000003245 coal Substances 0.000 claims abstract description 35
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 31
- 238000001035 drying Methods 0.000 claims abstract description 24
- 238000005406 washing Methods 0.000 claims abstract description 24
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 claims abstract description 19
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 16
- 230000007935 neutral effect Effects 0.000 claims abstract description 16
- 239000000843 powder Substances 0.000 claims abstract description 16
- 238000011065 in-situ storage Methods 0.000 claims abstract description 10
- 238000001556 precipitation Methods 0.000 claims abstract description 10
- 238000004140 cleaning Methods 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims abstract description 8
- 239000008367 deionised water Substances 0.000 claims abstract description 8
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 8
- 239000012153 distilled water Substances 0.000 claims abstract description 8
- 238000000227 grinding Methods 0.000 claims abstract description 8
- 239000004570 mortar (masonry) Substances 0.000 claims abstract description 8
- 239000012299 nitrogen atmosphere Substances 0.000 claims abstract description 8
- 238000007873 sieving Methods 0.000 claims abstract description 8
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 21
- 229910001868 water Inorganic materials 0.000 claims description 15
- 238000003756 stirring Methods 0.000 claims description 14
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 7
- 238000009835 boiling Methods 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 7
- 239000012535 impurity Substances 0.000 claims description 7
- 229910017604 nitric acid Inorganic materials 0.000 claims description 7
- 238000000643 oven drying Methods 0.000 claims description 6
- 238000006555 catalytic reaction Methods 0.000 abstract description 6
- 238000005868 electrolysis reaction Methods 0.000 abstract description 3
- 238000007885 magnetic separation Methods 0.000 abstract description 3
- 238000001179 sorption measurement Methods 0.000 abstract description 3
- 238000004065 wastewater treatment Methods 0.000 abstract description 2
- 238000002156 mixing Methods 0.000 abstract 1
- 239000005416 organic matter Substances 0.000 abstract 1
- 230000000694 effects Effects 0.000 description 5
- 230000003197 catalytic effect Effects 0.000 description 4
- 239000002957 persistent organic pollutant Substances 0.000 description 4
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 229910017052 cobalt Inorganic materials 0.000 description 2
- 239000010941 cobalt Substances 0.000 description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000002306 biochemical method Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000013043 chemical agent Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/74—Iron group metals
- B01J23/745—Iron
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28002—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their physical properties
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- B01J35/00—Catalysts, in general, characterised by their form or physical properties
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- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/391—Physical properties of the active metal ingredient
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- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/03—Precipitation; Co-precipitation
- B01J37/031—Precipitation
- B01J37/035—Precipitation on carriers
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/288—Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
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Abstract
A preparation method of a catalyst for electrocatalytic degradation of organic wastewater relates to a preparation method of a wastewater treatment catalyst, and comprises the following steps of: washing the activated carbon carrier to be neutral by using deionized water, cooling, washing to be neutral, ultrasonically cleaning for 20min, and finally drying at 80 ℃ for later use; preparing a catalyst by an in-situ precipitation method: mixing the pretreated coal activated carbon powder and amorphous Fe78Si13B9Dispersing the powder into distilled water, placing the powder into a three-neck flask, and adding FeSO with the concentration of 1mol per liter under the protection of nitrogen atmosphere4.7H2Washing the O solution with ethanol for 5 times in an alternating way for 10-30 ml, drying the O solution in a vacuum oven for 12 hours, grinding the dried reaction product in a mortar, and sieving the ground reaction product with a 200-mesh sieve to obtain the coal-based activated carbon-loaded amorphous Fe78Si13B9Nano Fe3O4A catalyst. The invention prepares the catalyst integrating adsorption, catalysis, internal electrolysis and magnetic separation, and solves the problems that the catalyst is difficult to separate and recycle and the organic matter is efficiently removed.
Description
Technical Field
The invention relates to a preparation method of a catalyst for treating wastewater, in particular to a preparation method of a catalyst for electrocatalytic degradation of organic wastewater.
Background
In recent years, with the rapid development of industries such as paper making, plastics, textiles and the like, people synthesize more and more organic matters, wherein the types and the amount of organic pollutants which are difficult to biodegrade and pose serious threats to human health and ecological environment are increased increasingly, and a large amount of organic pollutant wastewater is generated along with the organic pollutants. Most of the organic matters in the wastewater are refractory substances, and the effluent of refractory organic wastewater treated by the traditional wastewater treatment methods such as a physical and chemical method and a biochemical method at the present stage is difficult to reach the standard, so the organic wastewater must be subjected to advanced treatment. Electrocatalysis in recent yearsThe method is used as a main advanced treatment method, and organic pollutants can be completely oxidized into CO without adding too many additional chemical agents2And H2O, mild reaction conditions, small occupied area, simple treatment equipment, strong controllability and the like, and is favored by researchers at home and abroad.
However, the conventional electrocatalysis method of the two-dimensional electrode system severely restricts the application of the electrocatalysis method due to the problems of small specific surface area, low electric energy utilization efficiency, high energy consumption, high operation and construction cost and the like. Compare in the electro-catalysis method of traditional two-dimensional electrode, electro-catalysis method of three-dimensional electrode has improved electro-catalysis's reaction area, treatment effeciency and electric energy utilization efficiency. The key technology of the electrocatalysis method of the three-dimensional electrode lies in the catalyst and the activity effect.
At present, the research on the active carbon supported metal ion catalyst becomes a research hotspot in the field. The patent application with publication number CN 104383953 a discloses an activated carbon-supported cobalt catalyst, and a preparation method and application thereof, the method has harsh preparation conditions, hydrogen peroxide is needed when wastewater is degraded, the wastewater degradation cost is greatly increased, the effect is low, and secondary pollution is easily generated because cobalt belongs to toxic metal. The preparation method of the activated carbon supported catalyst for electrocatalytic degradation of organic wastewater with publication No. CN 105457643A has the advantages of high production cost due to the use of rare earth metal, difficult recovery of the catalyst and easy generation of secondary pollution. Therefore, the development or optimization of the prior art to prepare a novel catalyst which is low in cost, short in time consumption, renewable, recyclable and free of secondary pollution is a major problem in the field at present.
Disclosure of Invention
The invention aims to provide a preparation method of a catalyst for electrocatalytic degradation of organic wastewater78Si13B9And magnetic nano Fe3O4Combining, synthesizing coal activated carbon loaded amorphous Fe by an in-situ precipitation method78Si13B9Nano Fe3O4Catalyst, preparing the catalyst integrating adsorption, catalysis, internal electrolysis and magnetic separationThe method solves the problems that the catalyst is difficult to separate and recycle and the organic matters are removed efficiently.
The purpose of the invention is realized by the following technical scheme:
a preparation method of a catalyst for electrocatalytic degradation of organic wastewater is used for preparing novel high-catalytic-activity coal-based activated carbon-loaded amorphous Fe78Si13B9Nano Fe3O4A method of catalyzing, the method comprising the process of:
(1) pretreating a coal activated carbon carrier: washing the activated carbon carrier to be neutral by using deionized water, removing ash and other impurities on the surface, and drying at 100 ℃; boiling in 1mol/L dilute nitric acid for 30min, cooling, washing to neutrality, ultrasonically cleaning for 20min, and oven drying at 80 deg.C;
(2) preparing a catalyst by an in-situ precipitation method: firstly, the pretreated coal activated carbon powder and amorphous Fe78Si13B9Dispersing the powder into distilled water, placing the powder into a three-neck flask, and adding FeSO with the concentration of 1mol per liter under the protection of nitrogen atmosphere4.7H210-30 ml of O solution, and heating the solution to 75-95 ℃ through water bath; then dropwise adding 15-35 ml of NaOH solution with the concentration of 3 mol per liter at the speed of 5 ml/min, stirring while dropwise adding, and after dropwise adding, fully stirring for 5 min; followed by the addition of NaNO at a concentration of 1mol/l35-30 ml of solution, and keeping the system to react for 2 hours; finally, magnetically separating out a reaction product, alternately washing the obtained reaction product with water and ethanol for 5 times, drying the reaction product in a drying oven in vacuum for 12 hours, grinding the dried reaction product in a mortar, and sieving the ground reaction product through a 200-mesh sieve to obtain the coal-based activated carbon-loaded amorphous Fe78Si13B9Nano Fe3O4A catalyst.
According to the preparation method of the catalyst for electrocatalytic degradation of organic wastewater, the addition amount of the pretreated coal-based activated carbon powder is 30-200 g.
The preparation method of the catalyst for electrocatalytic degradation of organic wastewater comprises the step of preparing amorphous Fe78Si13B9The adding amount of the powder is 20-200 g。
The invention has the advantages and effects that:
1. the coal-based activated carbon of the invention loads amorphous Fe78Si13B9Nano Fe3O4Catalyst, which integrates the adsorptivity of coal-based activated carbon and amorphous Fe78Si13B9High catalytic activity and nano Fe3O4The catalyst has the characteristics of integration of adsorption, catalysis, internal electrolysis and magnetic separation, can be separated and recovered, and can efficiently remove organic matters without secondary pollution.
2. Compared with the sol-gel preparation of the activated carbon supported catalyst, the preparation method of the invention adopts an in-situ precipitation method, has simple process, does not need high-temperature roasting, simultaneously has low price of materials required by experiments, does not need expensive materials such as rare metals and the like, and has low production cost.
3. The method has the advantages of simple operation, easy equipment acquisition, simple process flow and low investment cost, and the prepared catalyst does not need to be additionally added with other oxidants in the process of degrading organic wastewater through electrocatalysis, thereby being beneficial to large-scale industrialized application.
Detailed Description
The present invention will be described in detail with reference to examples.
Example 1
The invention provides a method for preparing novel high catalytic activity coal-based activated carbon-loaded amorphous Fe78Si13B9Nano Fe3O4The method of the catalyst comprises the following specific steps:
(1) pretreating a coal activated carbon carrier: washing the activated carbon carrier to be neutral by using deionized water, removing ash and other impurities on the surface, and drying at 100 ℃. Boiling in 1mol/L dilute nitric acid for 30min, cooling, washing to neutrality, ultrasonically cleaning for 20min, and oven drying at 80 deg.C.
(2) Preparing a catalyst by an in-situ precipitation method: firstly, the pretreated coal activated carbon powder (the adding amount is 30 g) and amorphous Fe78Si13B9Powder (adding amount is 30 g)) Dispersing in distilled water, placing in a three-neck flask, adding FeSO with concentration of 1mol per liter under the protection of nitrogen atmosphere4.7H210 ml of O solution, and heating the solution to 75 ℃ through water bath; then, 20 ml of NaOH solution with the concentration of 3 mol per liter is dripped at the speed of 5 ml/min, stirring is carried out while dripping, and after dripping is finished, stirring is carried out for 5 min; followed by the addition of NaNO at a concentration of 1mol/l3Keeping the system reacting for 2 hours with 10 ml of solution; and finally, magnetically separating out a reaction product, alternately washing the obtained reaction product for 5 times by using water and ethanol until the pH of the solution is neutral, drying the reaction product in a drying oven in vacuum for 12 hours, grinding the dried reaction product in a mortar, and sieving the ground reaction product by using a 200-mesh sieve to obtain the coal-based activated carbon-loaded amorphous Fe78Si13B9Nano Fe3O4A catalyst.
Example 2
The invention provides a method for preparing novel high catalytic activity coal-based activated carbon-loaded amorphous Fe78Si13B9Nano Fe3O4The method of the catalyst comprises the following specific steps:
(1) pretreating a coal activated carbon carrier: washing the activated carbon carrier to be neutral by using deionized water, removing ash and other impurities on the surface, and drying at 100 ℃. Boiling in 1mol/L dilute nitric acid for 30min, cooling, washing to neutrality, ultrasonically cleaning for 20min, and oven drying at 80 deg.C.
(2) Preparing a catalyst by an in-situ precipitation method: firstly, the pretreated coal activated carbon powder (the adding amount is 100 g) and amorphous Fe78Si13B9Dispersing the powder (the addition amount is 150 g) into distilled water, placing the powder into a three-neck flask, and adding FeSO with the concentration of 1mol per liter under the protection of nitrogen atmosphere4.7H220 ml of O solution, and heating the solution to 80 ℃ through water bath; then, 25 milliliters of NaOH solution with the concentration of 3 mol per liter is dripped at the speed of 5 milliliters per minute, the dripping and the stirring are carried out simultaneously, and after the dripping is finished, the stirring is carried out for 5 minutes again; followed by the addition of NaNO at a concentration of 1mol/l315 ml of solution, and keeping the system to react for 2 hours; finally, the reaction product is separated out through magnetic separation,alternately washing the obtained reaction product with water and ethanol for 5 times until the pH of the solution is neutral, drying the solution in a drying oven for 12 hours in vacuum, grinding the dried reaction product in a mortar, and sieving the ground reaction product with a 200-mesh sieve to obtain the coal-based activated carbon-loaded amorphous Fe78Si13B9Nano Fe3O4A catalyst.
Example 3
The invention provides a method for preparing novel high catalytic activity coal-based activated carbon-loaded amorphous Fe78Si13B9Nano Fe3O4The method of the catalyst comprises the following specific steps:
(1) pretreating a coal activated carbon carrier: washing the activated carbon carrier to be neutral by using deionized water, removing ash and other impurities on the surface, and drying at 100 ℃. Boiling in 1mol/L dilute nitric acid for 30min, cooling, washing to neutrality, ultrasonically cleaning for 20min, and oven drying at 80 deg.C.
(2) Preparing a catalyst by an in-situ precipitation method: firstly, the pretreated coal activated carbon powder (the adding amount is 150 g) and amorphous Fe78Si13B9Dispersing the powder (the adding amount is 200 g) into distilled water, placing the powder into a three-neck flask, and adding FeSO with the concentration of 1mol per liter under the protection of nitrogen atmosphere4.7H230 ml of O solution, and heating the solution to 95 ℃ through water bath; then, 30 ml of NaOH solution with the concentration of 3 mol per liter is dripped at the speed of 5 ml/min, stirring is carried out while dripping, and after dripping is finished, stirring is carried out for 5 min; followed by the addition of NaNO at a concentration of 1mol/l3Keeping the system reacting for 2 hours with 20 ml of solution; and finally, magnetically separating out a reaction product, alternately washing the obtained reaction product for 5 times by using water and ethanol until the pH of the solution is neutral, drying the reaction product in a drying oven in vacuum for 12 hours, grinding the dried reaction product in a mortar, and sieving the ground reaction product by using a 200-mesh sieve to obtain the coal-based activated carbon-loaded amorphous Fe78Si13B9Nano Fe3O4A catalyst.
Claims (3)
1. Amorphous Fe loaded on coal-based activated carbon78Si13B9Nano Fe3O4A method for preparing a catalyst, the method comprising:
(1) pretreating a coal activated carbon carrier: washing the activated carbon carrier to be neutral by using deionized water, removing ash and other impurities on the surface, and drying at 100 ℃; boiling in 1mol/L dilute nitric acid for 30min, cooling, washing to neutrality, ultrasonically cleaning for 20min, and oven drying at 80 deg.C;
(2) preparing a catalyst by an in-situ precipitation method: firstly, 30 g of the pretreated coal activated carbon powder and 30 g of amorphous Fe78Si13B9Dispersing the powder into distilled water, placing the powder into a three-neck flask, and adding FeSO with the concentration of 1mol per liter under the protection of nitrogen atmosphere4· 7H210 ml of O solution, and heating the solution to 75 ℃ through water bath; then, 20 ml of NaOH solution with the concentration of 3 mol per liter is dripped at the speed of 5 ml/min, stirring is carried out while dripping, and after dripping is finished, stirring is carried out for 5 min; followed by the addition of NaNO at a concentration of 1mol/l3Keeping the system reacting for 2 hours with 10 ml of solution; and finally, magnetically separating out a reaction product, alternately washing the obtained reaction product for 5 times by using water and ethanol until the pH of the solution is neutral, drying the reaction product in a drying oven in vacuum for 12 hours, grinding the dried reaction product in a mortar, and sieving the ground reaction product by using a 200-mesh sieve to obtain the coal-based activated carbon-loaded amorphous Fe78Si13B9Nano Fe3O4A catalyst.
2. Amorphous Fe loaded on coal-based activated carbon78Si13B9Nano Fe3O4A method for preparing a catalyst, the method comprising:
(1) pretreating a coal activated carbon carrier: washing the activated carbon carrier to be neutral by using deionized water, removing ash and other impurities on the surface, drying at 100 ℃, boiling in 1mol/L dilute nitric acid for 30min, cooling, washing to be neutral, ultrasonically cleaning for 20min, and finally drying at 80 ℃ for later use;
(2) preparing a catalyst by an in-situ precipitation method: first, 100 g of the above pretreated coal-based activated carbon powder and 150 g of coal-based activated carbon powder were mixed with each otherCrystalline Fe78Si13B9Dispersing the powder into distilled water, placing the powder into a three-neck flask, and adding FeSO with the concentration of 1mol per liter under the protection of nitrogen atmosphere4· 7H220 ml of O solution, and heating the solution to 80 ℃ through water bath; then, 25 milliliters of NaOH solution with the concentration of 3 mol per liter is dripped at the speed of 5 milliliters per minute, the dripping and the stirring are carried out simultaneously, and after the dripping is finished, the stirring is carried out for 5 minutes again; followed by the addition of NaNO at a concentration of 1mol/l315 ml of solution, and keeping the system to react for 2 hours; and finally, magnetically separating out a reaction product, alternately washing the obtained reaction product for 5 times by using water and ethanol until the pH of the solution is neutral, drying the reaction product in a drying oven in vacuum for 12 hours, grinding the dried reaction product in a mortar, and sieving the ground reaction product by using a 200-mesh sieve to obtain the coal-based activated carbon-loaded amorphous Fe78Si13B9Nano Fe3O4A catalyst.
3. Amorphous Fe loaded on coal-based activated carbon78Si13B9Nano Fe3O4A method for preparing a catalyst, the method comprising:
(1) pretreating a coal activated carbon carrier: washing the activated carbon carrier to be neutral by using deionized water, removing ash and other impurities on the surface, and drying at 100 ℃; boiling in 1mol/L dilute nitric acid for 30min, cooling, washing to neutrality, ultrasonically cleaning for 20min, and oven drying at 80 deg.C;
(2) preparing a catalyst by an in-situ precipitation method: firstly, 150 g of the pretreated coal activated carbon powder and 200 g of amorphous Fe78Si13B9Dispersing the powder into distilled water, placing the powder into a three-neck flask, and adding FeSO with the concentration of 1mol per liter under the protection of nitrogen atmosphere4· 7H230 ml of O solution, and heating the solution to 95 ℃ through water bath; then, 30 ml of NaOH solution with the concentration of 3 mol per liter is dripped at the speed of 5 ml/min, stirring is carried out while dripping, and after dripping is finished, stirring is carried out for 5 min; followed by the addition of NaNO at a concentration of 1mol/l3Keeping the system reacting for 2 hours with 20 ml of solution; finally, the reaction product is separated out through magnetic separationAlternately washing the obtained reaction product with water and ethanol for 5 times until the pH of the solution is neutral, drying the reaction product in a drying oven for 12 hours in vacuum, grinding the dried reaction product in a mortar, and sieving the ground reaction product with a 200-mesh sieve to obtain the coal-based activated carbon-loaded amorphous Fe78Si13B9Nano Fe3O4A catalyst.
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