CN113019317A - Bimetal-loaded activated carbon high-performance adsorbent and preparation method and application thereof - Google Patents
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- B—PERFORMING OPERATIONS; TRANSPORTING
- 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
- B01J20/02—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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- B—PERFORMING OPERATIONS; TRANSPORTING
- 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
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0211—Compounds of Ti, Zr, Hf
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- B—PERFORMING OPERATIONS; TRANSPORTING
- 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
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0225—Compounds of Fe, Ru, Os, Co, Rh, Ir, Ni, Pd, Pt
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- B—PERFORMING OPERATIONS; TRANSPORTING
- 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
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/34—Regenerating or reactivating
- B01J20/3416—Regenerating or reactivating of sorbents or filter aids comprising free carbon, e.g. activated carbon
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- B—PERFORMING OPERATIONS; TRANSPORTING
- 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
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/34—Regenerating or reactivating
- B01J20/345—Regenerating or reactivating using a particular desorbing compound or mixture
- B01J20/3475—Regenerating or reactivating using a particular desorbing compound or mixture in the liquid phase
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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
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
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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
- C02F2101/306—Pesticides
Abstract
The invention discloses a preparation method of a high-performance adsorbent loaded with bimetallic cobalt/zirconium activated carbon and application of the adsorbent in organic pesticide wastewater treatment. The method comprises the steps of taking porous activated carbon with large specific surface area as a carrier, loading cobalt ions and zirconium ions on the activated carbon by a solution impregnation method, then stably fixing two metal ions on the inner surface and the outer surface of pores of the activated carbon by high-temperature calcination, and finally grinding calcined solids into powder by a grinding mode to obtain the loaded bimetallic activated carbon high-performance adsorbent Co/Zr @ AC. The prepared adsorbent has high stability and can effectively remove the organic pesticide atrazine in water. The adsorbent can be repeatedly used after desorption and regeneration, and the removal rate of the loaded bimetallic activated carbon repeatedly used for 5 times on the atrazine is still higher than 93%. The prepared loaded bimetallic active carbon is a promising environment functional material and has higher practicability and popularization in the field of organic wastewater treatment.
Description
Technical Field
The invention belongs to the technical field of material technology and sewage treatment, and particularly relates to a preparation method of a bimetallic cobalt/zirconium loaded activated carbon high-performance adsorbent and a technology for removing refractory organic pesticide atrazine.
Background
In the worldwide agriculture, atrazine can prevent and remove broadleaf weeds and grassy weeds, can also be used as a non-selective herbicide on fallow land and non-farmland land, and has the annual usage amount of 7-9 ten thousand tons in the whole world. Due to the limitations and unjustified use of technology, the amount of atrazine entering the environment is considerable. Calculated, the area of the land polluted by atrazine in China exceeds 1.0 multiplied by 1010hm. Since atrazine destroys the reproductive and immune systems of mammals, crustaceans, reptiles and amphibians, and even harms human health. In view of the wide use of atrazine, environmental stability and influence on the ecosystem, the research on how to remove atrazine in the environment is the focus of the current research.
At present, the technology for treating atrazine in water at home and abroad can be divided into a physical method, a chemical method and a biological method. The physical method has short treatment period, is convenient and quick, but cannot fundamentally remove pollutants, and can generate secondary pollution. The chemical method can realize the efficient and rapid degradation of atrazine, but the operation cost is high, and certain limitations exist in practical application. The biological method is simple to operate, has small influence on the environment, and has relatively long degradation period. Therefore, the development of novel organic pesticide treatment materials and techniques is of particular importance.
The activated carbon has large specific surface area, porous structure and abundant surface functional groups and is often used for removing waterThe various pollutants of (2) have been reported to remove atrazine from water by using activated carbon, but the prior results show that the removal of atrazine does not reach the expected effect, and the problems of difficult reutilization exist. In order to improve the removal capability of the activated carbon, modification treatment of the activated carbon by a technical means is a research hotspot at present, and many scholars do many researches. For example, the document "preparation of activated carbon supported Co-Mo bimetallic desulfurization catalyst by impregnation precipitation" (journal of Fuel chemistry, 2012, 40(10):1252-2. Patent CN109967041B 'bimetal modified magnetic biomass active carbon adsorbent, preparation method thereof and application in wastewater treatment' discloses a preparation method of bimetal Fe/Mg loaded active carbon, and is applied to treatment of malachite green dye. The literature 'research on removing Trichloroethylene (TCE) in water by using bimetallic activated carbon loaded with nano zero-valent iron/palladium (ZVI/Pd)' (water purification technology, 2013, 32(1):67-73) researches on loading nano zero-valent iron/palladium on activated carbon and removing the trichloroethylene in the water. The document "Mn-Ce bimetallic/activated carbon catalytic ozonation treatment of methylene blue wastewater" (industrial water treatment, 2019, 39(8):60-65) prepares bimetallic Mn-Ce loaded activated carbon material and is used for treating methylene blue wastewater. The above documents have some researches on the treatment of pollutants with the bimetal loaded activated carbon material, but the preparation cost of the bimetal loaded activated carbon is high, the process is complex, the reuse rate is low, meanwhile, the method has a certain deficiency in removing pollutants difficult to degrade, especially organic pesticides, and the removal effect of the bimetal loaded activated carbon is still to be further improved.
Disclosure of Invention
The invention aims to solve the technical problem of overcoming the defects of the prior art and provides a preparation method of a high-performance adsorbent loaded with bimetallic cobalt/zirconium activated carbon and an application of the high-performance adsorbent in removing difficultly-degradable organic pesticide atrazine. In order to achieve the above purpose, the invention provides a preparation method of a high-performance adsorbent loaded with bimetallic activated carbon, which comprises the following steps:
(1) active carbon pretreatment: soaking activated carbon powder sieved by a standard sample sieve of 50-150 meshes in 0.5mol/L sodium hydroxide solution for 24 hours, preparing the activated carbon and the sodium hydroxide solution according to the solid-to-liquid ratio (g: mL) of (1-4): 10, washing the filtered activated carbon with ultrapure water to be neutral, and drying at the temperature of 60-95 ℃; and then, according to the solid-liquid ratio (g: mL) of (1-4) to 10, soaking the dried activated carbon in 1.0mol/L hydrochloric acid solution for 24 hours, washing the filtered activated carbon to be neutral by using ultrapure water, and drying at the temperature of 60-95 ℃.
(2) Bimetallic loaded activated carbon: dipping the pretreated activated carbon into a bimetal mixed liquid containing cobalt ions and zirconium ions according to a solid-liquid ratio (g: mL) of (1-6): 100 by a solution dipping method, stirring at a rotating speed of 30-100 rpm for 2-12 hours, filtering the activated carbon, and drying at the temperature of 60-95 ℃ to obtain the loaded bimetal activated carbon, wherein the bimetal mixed liquid is prepared according to the mass ratio of the cobalt ions to the zirconium ions of 0.2-6.0.
(3) And (3) high-temperature calcination of loaded activated carbon: calcining the loaded bimetallic activated carbon obtained in the step at 200-800 ℃ for 2-7 hours, cooling, grinding, and sieving by a 50-150-target standard sample sieve to obtain the high-performance adsorbent Co/Zr @ AC of the loaded bimetallic activated carbon.
The invention provides a technology for removing difficultly degraded pesticide atrazine by using the loaded bimetallic activated carbon, which is characterized by comprising the following steps of: adjusting the pH value of the atrazine solution to 2-11, mixing the loaded bimetallic activated carbon and the atrazine solution according to the mode that the mass ratio (g: g) of the loaded bimetallic activated carbon to the atrazine is (2-20): 1, and reacting for 20-180 minutes at the temperature of 15-45 ℃.
The invention also provides a technology for desorbing and regenerating the reacted loaded bimetallic activated carbon, which is characterized in that: filtering the reacted loaded bimetallic activated carbon by a 0.45-micrometer filter membrane, sequentially washing the reacted loaded bimetallic activated carbon for 3-5 times by 80-99.5% of methanol and ultrapure water, and drying the obtained product for 10-24 hours at the temperature of 60-95 ℃ to obtain the desorbed and regenerated loaded bimetallic activated carbon. The desorbed and regenerated loaded bimetallic activated carbon is used for removing atrazine, and after the loaded bimetallic activated carbon is repeatedly used for 5 times, the removal rate of the loaded bimetallic activated carbon to the atrazine is still higher than 93%.
The invention utilizes the solution impregnation and high-temperature calcination technology, selects the active carbon with larger specific surface area and abundant surface functional groups as a carrier, and loads the bimetallic cobalt/zirconium on the active carbon to prepare the loaded bimetallic active carbon high-performance adsorbent, thereby improving the removal performance of the active carbon on the difficultly-degraded organic pesticide atrazine. Meanwhile, the use times of the materials are improved and the operating cost of the technology is effectively reduced through desorption regeneration of the methanol and the ultrapure water.
The invention has the characteristics that: the active carbon selected by the invention has better adsorption capacity, and the used bimetallic cobalt/zirconium composite metal has strong oxidation-reduction property, so that the prepared adsorbent for loading the bimetallic active carbon has stronger adsorption capacity and oxidation-reduction property on pollutants, and the removal performance of the active carbon on organic pollutants is improved. The loaded bimetallic activated carbon high-performance adsorbent has the highest atrazine removal rate of 97 percent, can be repeatedly used for many times, and provides a novel material and a feasible technical method for removing organic pesticides in water in China.
Drawings
Fig. 1 is a scanning electron micrograph and an energy chromatogram of the bimetallic-loaded activated carbon.
Fig. 2 is a schematic diagram of the relationship between the adsorption capacity of the loaded bimetallic activated carbon to atrazine and the change of the dipping time of the bimetallic solution in embodiment 1 of the present invention.
Fig. 3 is a schematic diagram of the removal rate of atrazine by the addition amount of the loaded bimetallic activated carbon in embodiment 2 of the invention.
Fig. 4 is a schematic diagram of the reuse times of the loaded bimetallic activated carbon to the atrazine removal rate in example 3 of the present invention.
Detailed Description
The invention is further described with reference to the following figures and examples.
Example 1:
a preparation method of a high-performance adsorbent loaded with bimetallic activated carbon comprises the following steps:
(1) active carbon pretreatment: soaking activated carbon powder sieved by a 100-mesh standard sample sieve in a sodium hydroxide solution with the concentration of 0.5mol/L for 24 hours, washing the filtered solid with ultrapure water to be neutral, and then drying at 80 ℃; soaking the dried activated carbon in 1.0mol/L hydrochloric acid solution for 24 hours, washing the filtered solid to be neutral by using ultrapure water, and drying at 80 ℃.
(2) Active carbon loaded bimetallic: soaking 1g of pretreated activated carbon in 100mL of cobalt/zirconium bimetal mixed solution by a solution soaking method, wherein the mass fraction ratio of cobalt ions to zirconium ions is 1:1, stirring at the rotating speed of 80rpm for 3, 5, 7, 9 and 12 hours respectively, filtering the activated carbon, and drying at the temperature of 80 ℃ to obtain the loaded bimetal activated carbon.
(3) And (3) high-temperature calcination of loaded activated carbon: calcining the loaded bimetallic activated carbon obtained in the step at 400 ℃ for 3 hours, cooling, grinding, and screening by using a 100-mesh standard sample sieve to obtain the loaded bimetallic activated carbon high-performance adsorbent.
The loaded bimetallic activated carbon is used for removing the atrazine which is a pesticide difficult to degrade, and the specific operation steps are as follows: preparing 50mL of an atrazine water sample with the concentration of 10mg/L, adjusting the pH of the solution to be 6.0, adding 60mg/L of the loaded bimetallic activated carbon, reacting for 150 minutes in a constant-temperature water bath shaker at the rotating speed of 100rpm, taking a proper amount of the water sample, filtering the water sample by using a filter membrane, and measuring the residual amount of the atrazine in the water sample by using a high performance liquid chromatograph. The result shows that the adsorption capacity of the material to the atrazine can reach 117.23mg/g at most.
Example 2:
a preparation method of a high-performance adsorbent loaded with bimetallic activated carbon comprises the following steps:
(1) active carbon pretreatment: soaking activated carbon powder sieved by a 100-mesh standard sample sieve in a sodium hydroxide solution with the concentration of 0.5mol/L for 24 hours, washing the filtered solid with ultrapure water to be neutral, and then drying at the temperature of 95 ℃; soaking the dried activated carbon in 1.0mol/L hydrochloric acid solution for 24 hours, washing the filtered solid to be neutral by using ultrapure water, and drying at 95 ℃.
(2) Active carbon loaded bimetallic: soaking 1g of pretreated activated carbon in 100mL of cobalt/zirconium bimetal mixed solution, wherein the mass fraction ratio of cobalt ions to zirconium ions is 1:2, stirring at the rotating speed of 100rpm for 5 hours, filtering the activated carbon, and drying at the temperature of 95 ℃ to obtain the loaded bimetal activated carbon.
(3) And (3) high-temperature calcination of loaded activated carbon: calcining the loaded bimetallic activated carbon obtained in the step at 500 ℃ for 4 hours, cooling, then grinding the calcined loaded bimetallic activated carbon into a mortar, and screening by using a 100-mesh standard sample sieve to obtain the loaded bimetallic activated carbon high-performance adsorbent.
The loaded bimetallic activated carbon high-performance adsorbent is used for removing the difficultly degraded pesticide atrazine, and the specific operation steps are as follows: preparing 50mL of an atrazine water sample with the concentration of 10mg/L, adjusting the pH of the solution to be 4.0, respectively adding 20, 40, 60, 80, 100, 120, 140, 160 and 180mg/L of the loaded bimetallic activated carbon, reacting for 180 minutes in a constant-temperature water bath shaker at the rotating speed of 100rpm, filtering a proper amount of the water sample through a filter membrane, measuring the residual amount of the atrazine in the water sample by using a high performance liquid chromatograph, and calculating the removal rate. The result shows that the highest removal rate of the atrazine can reach 97.45 percent.
Example 3:
filtering the mixed solution adsorbed in the embodiment 2 by a filter membrane of 0.45um to obtain the loaded bimetallic activated carbon after reaction, then sequentially washing the mixed solution by 90.5% methanol and ultrapure water for 5 times to remove the solvent and unreacted atrazine, and then drying the mixed solution for 24 hours at the temperature of 95 ℃ to obtain the loaded bimetallic activated carbon after desorption and regeneration.
The method for removing the difficultly degraded pesticide atrazine by using the desorbed and regenerated loaded bimetallic activated carbon high-performance adsorbent comprises the following specific operation steps: preparing 50mL of an atrazine water sample with the concentration of 10mg/L, adjusting the pH of the solution to be 4.0, adjusting the adding amount of the loaded bimetallic activated carbon to be 180mg/L, reacting for 180 minutes in a constant-temperature water bath shaker at the rotating speed of 100rpm, taking a proper amount of the water sample, filtering the water sample by using a filter membrane, measuring the residual amount of the atrazine in the water sample by using a high performance liquid chromatograph, calculating the removal rate, and repeating the experiment according to the steps. The result shows that after the adsorbent is repeatedly used for 5 times, the removal rate of the high-performance adsorbent loaded with the bimetallic activated carbon on the atrazine is still higher than 93%.
Claims (6)
1. A preparation method of a bimetal loaded activated carbon high-performance adsorbent is characterized by comprising the following steps:
(1) immersing the pretreated activated carbon powder into a bimetal mixed solution containing cobalt ions and zirconium ions, stirring at the rotating speed of 30-100 rpm, filtering the immersed activated carbon after 2-12 hours, and drying at the temperature of 60-95 ℃;
(2) calcining the activated carbon obtained in the step (1) at 200-800 ℃ for 2-7 hours, cooling, grinding and sieving by a 50-150-target standard sample sieve to obtain the high-performance adsorbent Co/Zr @ AC loaded with the bimetallic activated carbon.
2. The method of claim 1, wherein: in the step (1), the cobalt ion-containing solution can be Co (NO)3)2·6H2O、CoCl2、CoSO4The zirconium ion-containing solution can be Zr (NO)3)4·5H2O、Zr(SO4)2The preparation method comprises the following steps of (1) preparing a bimetal mixed solution, wherein the weight ratio of cobalt ions to zirconium ions is 0.2-6.0, and soaking the activated carbon and the bimetal mixed solution according to the solid-liquid ratio (g: mL) of (1-6): 100.
3. The loaded bimetallic activated carbon high-performance adsorbent according to any one of claims 1 to 2, characterized in that the adsorbent can be used for removing refractory organic pesticide atrazine in water.
4. The loaded bimetal activated carbon high-performance adsorbent as claimed in claim 3, wherein the step of removing the refractory organic pesticide atrazine from the water by the adsorbent is as follows: adjusting the pH value of the atrazine solution to 2-11, mixing the loaded bimetallic activated carbon and the atrazine solution according to the mode that the mass ratio (g: g) of the loaded bimetallic activated carbon to the atrazine is (2-20): 1, and reacting for 20-180 minutes at the temperature of 15-45 ℃.
5. The loaded bi-metallic activated carbon high performance sorbent of claim 4, wherein: and filtering the reacted loaded bimetallic activated carbon by a 0.45-micrometer filter membrane, repeatedly cleaning the reacted loaded bimetallic activated carbon by methanol and ultrapure water in sequence, and drying the washed loaded bimetallic activated carbon for 10 to 24 hours at the temperature of between 60 and 95 ℃ to obtain the desorbed and regenerated loaded bimetallic activated carbon.
6. The use of the loaded bi-metallic activated carbon high performance sorbent of claim 5, wherein: the content of the methanol in the cleaning liquid is 80-99.5%, the cleaning times are 3-5 times, and the ultrapure water cleaning times are 3-5 times.
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| CN113577940A (en) * | 2021-08-21 | 2021-11-02 | 珠海格力电器股份有限公司 | Filling type filter screen, air purifier and regeneration method of filter material |
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Application publication date: 20210625 |