Preparation method of activated carbon supported iron-carbon catalyst

The preparation of activated carbon-supported iron-carbon catalyst by impregnation and precipitation method solves the problem of catalyst instability in HCO technology, achieves efficient removal of odor substances in water, and the preparation method is simple and low cost.

CN122098571APending Publication Date: 2026-05-29GUANGZHOU WATER SUPPLY CO +1
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
GUANGZHOU WATER SUPPLY CO
Filing Date
2026-04-07
Publication Date
2026-05-29

AI Technical Summary

Technical Problem

The catalysts in existing HCO technologies have unstable structures and catalytic performance, making it difficult to efficiently remove odor-causing substances such as geosmin and 2-methylisoborneol from water.

Method used

An activated carbon-supported iron-carbon catalyst was prepared by impregnation and precipitation. The catalytic properties of Fe3C were utilized, and ozone oxidation was combined to remove odorous substances from the water.

Benefits of technology

It achieves a high removal rate of over 90% for geosmin and 2-methylisoborneol, and the preparation method is simple, low-cost, green and safe.

✦ Generated by Eureka AI based on patent content.

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Abstract

The application relates to a preparation method of an activated carbon loaded iron-carbon catalyst, and belongs to the field of drinking water purification and wastewater pollution treatment. The application aims to solve the problems of unstable catalyst structure and unstable catalytic performance in the existing HCO technology, and cannot meet the removal requirements of smell substances in water. The method comprises the following steps: 1, preparing a modified solution; 2, modifying activated carbon; and 3, preparing the activated carbon loaded iron-carbon catalyst through high-temperature pyrolysis. The application can synthesize catalytic materials through simple impregnation and precipitation, and can remove typical smell substances, geosmin and 2-methylisoborneol, in water through catalysis and ozone. The application can make up for the defects of unstable catalyst structure and unstable catalytic performance in the HCO technology, and has the advantages of simple preparation mode, low cost, green and safe catalyst and high practical popularization and application possibility.
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Description

Technical Field

[0001] This invention belongs to the field of drinking water purification and wastewater pollution control, and specifically relates to a method for preparing an activated carbon-supported iron-carbon catalyst. Background Technology

[0002] With the improvement of living standards, people have higher requirements for drinking water quality. In recent years, affected by global climate change and accelerated urbanization, eutrophication of water bodies has become increasingly serious, with algae proliferating in large quantities, leading to increasingly prominent pollution problems of odor-causing substances (such as geosmin and 2-methylisoborneol) and algal toxins in drinking water sources and aquaculture. Therefore, there is an urgent need to develop efficient, economical, and practical new water purification technologies to address the odor problem in drinking water.

[0003] Conventional water treatment processes struggle to efficiently remove odor-causing substances from water. While HCO3 technology holds significant potential for practical application, the use of standalone metal oxide and carbon catalysts exhibits structural and catalytic instability. Therefore, a catalyst is needed to remove typical odor-causing substances in water, such as geosmin and 2-methylisoborneol. Summary of the Invention

[0004] The purpose of this invention is to solve the problem that the catalyst structure and catalytic performance of existing HCO technology are unstable and cannot meet the requirements for removing odor substances in water, and to provide a method for preparing an activated carbon-supported iron-carbon catalyst.

[0005] This invention proposes a method for preparing an activated carbon-supported iron-carbon catalyst. This method can synthesize catalytic materials through simple impregnation and precipitation, catalyzing the removal of typical odor-causing substances geosmin and 2-methylisoborneol from water by ozone. This invention overcomes the shortcomings of unstable catalyst structure and catalytic performance in HCO technology, while also being simple to prepare, low in cost, and producing a green and safe catalyst, thus possessing high potential for practical application.

[0006] A method for preparing an activated carbon-supported iron-carbon catalyst is specifically carried out according to the following steps:

[0007] I. Preparation of the modified solution:

[0008] ① Preparation of Na3BTC solution: Add 1,3,5-pyromellitic acid and sodium hydroxide to deionized water, stir to dissolve, and obtain Na3BTC solution;

[0009] ② Preparation of FeCl3 solution: Add FeCl3 to deionized water, stir to dissolve, and obtain FeCl3 solution;

[0010] II. Modified Activated Carbon:

[0011] ① Dry the activated carbon powder, then immerse it in FeCl3 solution, stir while immersing, pour off the supernatant after precipitation, and then dry the resulting solid mixture.

[0012] ② Immerse the dried mixture in Na3BTC solution, stir while immersing, pour off the supernatant after precipitation, and then dry the resulting mixture to obtain modified activated carbon powder.

[0013] III. Preparation of activated carbon-supported iron-carbon catalysts by high-temperature pyrolysis:

[0014] ① Place the modified activated carbon powder into a corundum crucible, then place it in a tube furnace, heat it to the pyrolysis temperature under an inert gas atmosphere, keep it at the temperature, and finally cool it naturally to room temperature to obtain a black sample.

[0015] ② The black sample was washed until neutral, dried, and then ground into powder to obtain an activated carbon-supported iron-carbon catalyst.

[0016] Compared with the prior art, the present invention has the following advantages:

[0017] 1. The preparation method of the activated carbon supported iron-carbon catalyst prepared by this invention is simple, easy to operate, green and safe, with a short cycle and low cost, and is suitable for large-scale production applications;

[0018] 2. In the activated carbon-supported iron-carbon catalyst prepared by this invention, Fe is coated with carbon, and Fe3C is generated;

[0019] 3. The activated carbon-supported iron-carbon catalyst prepared in this invention can effectively catalyze ozone oxidation and remove odorous substances from water. Within 30 minutes, the removal rate of geosmin (GSM) and 2-methylisoborneol (2-MIB) can reach over 90%. Attached Figure Description

[0020] Figure 1 The experimental results of using activated carbon-supported iron-carbon catalysts prepared in Examples 1-3 to catalyze ozone oxidation to remove odor substances are shown in the left figure; the odor substance in the left figure is GSM, and the odor substance in the right figure is 2-MIB.

[0021] Figure 2 The XRD patterns of the activated carbon-supported iron-carbon catalysts prepared in Examples 1-2 are shown below.

[0022] Figure 3 This is a TEM image of the activated carbon-supported iron-carbon catalyst prepared in Example 2. Detailed Implementation

[0023] Specific Implementation Method 1: This implementation method is a method for preparing an activated carbon-supported iron-carbon catalyst, specifically completed according to the following steps:

[0024] I. Preparation of the modified solution:

[0025] ① Preparation of Na3BTC solution: Add 1,3,5-pyromellitic acid and sodium hydroxide to deionized water, stir to dissolve, and obtain Na3BTC solution;

[0026] ② Preparation of FeCl3 solution: Add FeCl3 to deionized water, stir to dissolve, and obtain FeCl3 solution;

[0027] II. Modified Activated Carbon:

[0028] ① Dry the activated carbon powder, then immerse it in FeCl3 solution, stir while immersing, pour off the supernatant after precipitation, and then dry the resulting solid mixture.

[0029] ② Immerse the dried mixture in Na3BTC solution, stir while immersing, pour off the supernatant after precipitation, and then dry the resulting mixture to obtain modified activated carbon powder.

[0030] III. Preparation of activated carbon-supported iron-carbon catalysts by high-temperature pyrolysis:

[0031] ① Place the modified activated carbon powder into a corundum crucible, then place it in a tube furnace, heat it to the pyrolysis temperature under an inert gas atmosphere, keep it at the temperature, and finally cool it naturally to room temperature to obtain a black sample.

[0032] ② The black sample was washed until neutral, dried, and then ground into powder to obtain an activated carbon-supported iron-carbon catalyst.

[0033] Specific Implementation Method Two: This implementation method differs from Specific Implementation Method One in that the concentration of the Na3BTC solution mentioned in step one ① is 20 mmol / L to 40 mmol / L. The other steps are the same as in Specific Implementation Method One.

[0034] Specific Implementation Method Three: This implementation method differs from Specific Implementation Method One or Two in that the concentration of the FeCl3 solution mentioned in step one, step two, is 10 mmol / L to 30 mmol / L. The other steps are the same as in Specific Implementation Method One or Two.

[0035] Specific Implementation Method Four: The difference between this implementation method and Specific Implementation Methods One to Three is that the soaking and stirring time in step two① is 1 to 2 hours. The other steps are the same as in Specific Implementation Methods One to Three.

[0036] Specific Implementation Method Five: This implementation method differs from Specific Implementation Methods One to Four in that: the precipitation time in step two① is 2h~4h; the drying temperature in step two① is 80℃, and the drying time is 8h~12h. Other steps are the same as in Specific Implementation Methods One to Four.

[0037] Specific Implementation Method Six: The difference between this implementation method and Specific Implementation Methods One to Five is that the soaking and stirring time in step two ② is 1 to 2 hours. The other steps are the same as in Specific Implementation Methods One to Five.

[0038] Specific Implementation Method Seven: This implementation method differs from Specific Implementation Methods One to Six in that: the precipitation time in step two ② is 2h~4h; the drying temperature in step two ② is 80℃, and the drying time is 8h~12h. Other steps are the same as in Specific Implementation Methods One to Six.

[0039] Specific Implementation Method Eight: This implementation method differs from Specific Implementation Methods One to Seven in that: the inert gas mentioned in step three ① is argon; the heating rate mentioned in step three ① is 2℃ / min to 5℃ / min. Other steps are the same as in Specific Implementation Methods One to Seven.

[0040] Specific Implementation Method Nine: This implementation method differs from Specific Implementation Methods One to Eight in that: the pyrolysis temperature in step three① is 600℃~800℃; the heat preservation time in step three① is 1h~2h. Other steps are the same as in Specific Implementation Methods One to Eight.

[0041] Specific Implementation Method Ten: This implementation method differs from Specific Implementation Methods One to Nine in that: in step three ②, the black sample is washed with deionized water until the washing solution is neutral; the drying temperature in step three ② is 80°C, and the drying time is 8h to 12h. Other steps are the same as in Specific Implementation Methods One to Nine.

[0042] The beneficial effects of the present invention are verified using the following embodiments:

[0043] Example 1: A method for preparing an activated carbon-supported iron-carbon catalyst, specifically comprising the following steps:

[0044] I. Preparation of the modified solution:

[0045] ① Preparation of Na3BTC solution: Add 1,3,5-pyromellitic acid and sodium hydroxide to deionized water, stir to dissolve, and obtain Na3BTC solution;

[0046] The concentration of the Na3BTC solution mentioned in step 1① is 30 mmol / L;

[0047] ② Preparation of FeCl3 solution: Add FeCl3 to deionized water, stir to dissolve, and obtain FeCl3 solution;

[0048] The concentration of the FeCl3 solution mentioned in step 1② is 20 mmol / L;

[0049] II. Modified Activated Carbon:

[0050] ① Dry the activated carbon powder, then immerse it in FeCl3 solution, stir while immersing, let it precipitate for 3 hours, pour off the supernatant, and then dry the resulting solid mixture.

[0051] The soaking and stirring time mentioned in step 2① is 1 hour;

[0052] The drying temperature described in step 2① is 80℃, and the drying time is 10 hours;

[0053] ② The dried mixture is immersed in Na3BTC solution, stirred and allowed to precipitate for 3 hours. The supernatant is then poured off and the resulting mixture is dried to obtain modified activated carbon powder.

[0054] The soaking and stirring time described in step 2② is 1 hour;

[0055] The drying temperature described in step 2② is 80℃, and the drying time is 10 hours;

[0056] III. Preparation of activated carbon-supported iron-carbon catalysts by high-temperature pyrolysis:

[0057] ① Place the modified activated carbon powder into a corundum crucible, then place it in a tube furnace, heat it to the pyrolysis temperature under an inert gas atmosphere, keep it at that temperature for 1 hour, and finally cool it naturally to room temperature to obtain a black sample.

[0058] The inert gas mentioned in step 3① is argon;

[0059] The heating rate mentioned in step 3① is 2℃ / min;

[0060] The pyrolysis temperature mentioned in step 3① is 800℃;

[0061] ② Wash the black sample with deionized water until the washing solution is neutral, dry it, and then grind it into powder to obtain activated carbon supported iron-carbon catalyst (800℃-Fe@C).

[0062] The drying temperature described in step 3② is 80℃, and the drying time is 10 hours.

[0063] Example 2: The difference between this example and Example 1 is that the pyrolysis temperature in step 3① is 700℃; and the activated carbon-supported iron-carbon catalyst (700℃-Fe@C) obtained in step 3② is different. All other steps and parameters are the same as in Example 1.

[0064] Example 3: The difference between this example and Example 1 is that the pyrolysis temperature in step 3.① is 600℃; and the activated carbon-supported iron-carbon catalyst (600℃-Fe@C) obtained in step 3.② is the same as in Example 1. All other steps and parameters are the same.

[0065] Application experiments for removing geosmin (GSM) and 2-methylisoborneol (2-MIB):

[0066] ① 0.2 g of the activated carbon-supported iron-carbon catalyst (800℃-Fe@C) prepared in Example 1 was added to 200 mL of polluted water containing 500 ng / L each of geosmin (GSM) and 2-methylisoborneol (2-MIB). Ozone was then added at a concentration of 2 mg / L, and the treatment lasted from 0 min to 30 min. The concentration of geosmin (GSM) in the water was detected using purge-trap-gas chromatography-mass spectrometry. The removal rate of GSM is shown in [the figure]. Figure 1 The 800Fe@C-O3 curve in the middle left figure shows the removal rate of 2-MIB. Figure 1 The 800Fe@C-O3 curve is shown in the middle right figure;

[0067] As a control, the activated carbon-supported iron-carbon catalyst (700℃-Fe@C) prepared in Example 1 was replaced with the activated carbon-supported iron-carbon catalyst prepared in Example 2. All other processes and parameters were the same as in ①. The GSM removal rate is shown in [reference needed]. Figure 1 The 700Fe@C-O3 curve is shown in the middle left figure; the removal rate of 2-MIB is shown in [the figure]. Figure 1 The 700Fe@C-O3 curve is shown in the middle right figure;

[0068] As a control, the activated carbon-supported iron-carbon catalyst (600℃-Fe@C) prepared in Example 1 was replaced with the activated carbon-supported iron-carbon catalyst prepared in Example 3. All other processes and parameters were the same as in ①. The GSM removal rate is shown in [reference needed]. Figure 1 The 600Fe@C-O3 curve is shown in the middle left figure; the removal rate of 2-MIB is shown in [the figure]. Figure 1 The 600Fe@C-O3 curve is shown in the middle right figure;

[0069] As a control, the activated carbon-supported iron-carbon catalyst prepared in Example 1 was omitted; all other processes and parameters were the same as in ①. The GSM removal rate is shown in [reference needed]. Figure 1 The middle left figure shows only the O3 curve; the removal rate of 2-MIB is shown in the figure. Figure 1 The onlyO3 curve is shown in the middle right figure.

[0070] Figure 1 The experimental results of using activated carbon-supported iron-carbon catalysts prepared in Examples 1-3 to catalyze ozone oxidation to remove odor substances are shown in the left figure; the odor substance in the left figure is GSM, and the odor substance in the right figure is 2-MIB.

[0071] Depend on Figure 1It can be seen that when the calcination temperature during catalyst preparation is 700-800℃, the removal effect on GSM and 2-MIB is the best, with a removal rate of over 90%.

[0072] Figure 2 The XRD patterns of the activated carbon-supported iron-carbon catalysts prepared in Examples 1-2 are shown below.

[0073] Depend on Figure 2 As can be seen from the PDF card, diffraction peaks of Fe3C and Fe can be observed at 700℃ and 800℃.

[0074] Figure 3 TEM image of the activated carbon-supported iron-carbon catalyst prepared in Example 2;

[0075] TEM images revealed the microstructure of iron-carbon nanoparticles calcined at 700℃, further confirming the presence of iron nanoparticles and graphitic carbon in the catalyst. The lattice spacings of 0.25 nm and 0.34 mm correspond to Fe3C (200) and graphitic carbon (002), respectively.

Claims

1. A method for preparing an activated carbon-supported iron-carbon catalyst, characterized in that... The preparation method is specifically carried out according to the following steps: I. Preparation of the modified solution: ① Preparation of Na3BTC solution: Add 1,3,5-pyromellitic acid and sodium hydroxide to deionized water, stir to dissolve, and obtain Na3BTC solution; ② Preparation of FeCl3 solution: Add FeCl3 to deionized water, stir to dissolve, and obtain FeCl3 solution; II. Modified activated carbon: ① Dry the activated carbon powder, then immerse it in FeCl3 solution, stir while immersing, pour off the supernatant after precipitation, and then dry the resulting solid mixture. ② Immerse the dried mixture in Na3BTC solution, stir while immersing, pour off the supernatant after precipitation, and then dry the resulting mixture to obtain modified activated carbon powder. III. Preparation of activated carbon-supported iron-carbon catalysts by high-temperature pyrolysis: ① Place the modified activated carbon powder into a corundum crucible, then place it in a tube furnace, heat it to the pyrolysis temperature under an inert gas atmosphere, keep it at the temperature, and finally cool it naturally to room temperature to obtain a black sample. ② The black sample was washed until neutral, dried, and then ground into powder to obtain an activated carbon-supported iron-carbon catalyst.

2. The method for preparing an activated carbon-supported iron-carbon catalyst according to claim 1, characterized in that... The concentration of the Na3BTC solution mentioned in step 1① is 20 mmol / L to 40 mmol / L.

3. The method for preparing an activated carbon-supported iron-carbon catalyst according to claim 1, characterized in that... The concentration of the FeCl3 solution mentioned in step 1② is 10 mmol / L to 30 mmol / L.

4. The method for preparing an activated carbon-supported iron-carbon catalyst according to claim 1, characterized in that... The soaking and stirring time mentioned in step 2① is 1h~2h.

5. The method for preparing an activated carbon-supported iron-carbon catalyst according to claim 1, characterized in that... The precipitation time mentioned in step 2① is 2h~4h; the drying temperature mentioned in step 2① is 80℃, and the drying time is 8h~12h.

6. The method for preparing an activated carbon-supported iron-carbon catalyst according to claim 1, characterized in that... The soaking and stirring time described in step 2② is 1h~2h.

7. The method for preparing an activated carbon-supported iron-carbon catalyst according to claim 1, characterized in that... The precipitation time in step 2② is 2h~4h; the drying temperature in step 2② is 80℃, and the drying time is 8h~12h.

8. The method for preparing an activated carbon-supported iron-carbon catalyst according to claim 1, characterized in that... The inert gas mentioned in step 3① is argon; the heating rate mentioned in step 3① is 2℃ / min~5℃ / min.

9. The method for preparing an activated carbon-supported iron-carbon catalyst according to claim 1, characterized in that... The pyrolysis temperature mentioned in step 3① is 600℃~800℃; the heat preservation time mentioned in step 3① is 1h~2h.

10. The method for preparing an activated carbon-supported iron-carbon catalyst according to claim 1, characterized in that... In step 3②, the black sample is washed with deionized water until the washing solution is neutral; the drying temperature in step 3② is 80℃ and the drying time is 8h~12h.