CN110550688B - By using CO2Method for removing phenols in water by activated charcoal activated persulfate degradation - Google Patents

By using CO2Method for removing phenols in water by activated charcoal activated persulfate degradation Download PDF

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CN110550688B
CN110550688B CN201910714119.8A CN201910714119A CN110550688B CN 110550688 B CN110550688 B CN 110550688B CN 201910714119 A CN201910714119 A CN 201910714119A CN 110550688 B CN110550688 B CN 110550688B
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CN110550688A (en
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陈彤
黄群星
孙晨
李晓东
严建华
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Zhejiang University ZJU
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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
    • C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
    • 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
    • C02F1/72—Treatment of water, waste water, or sewage by oxidation
    • C02F1/722—Oxidation by peroxides
    • 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
    • C02F1/72—Treatment of water, waste water, or sewage by oxidation
    • C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
    • 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
    • C02F2101/34—Organic compounds containing oxygen
    • C02F2101/345—Phenols

Abstract

The invention relates to a water treatment technology, and aims to provide a method for utilizing CO2A method for removing phenols in water by activated charcoal to activate persulfate for degradation. The catalyst is prepared by the following steps: placing microcrystalline cellulose in a tube furnace in N2Heating and carbonizing under the atmosphere to obtain unactivated biochar; continue at N2Raising the temperature to 800-950 ℃ in the atmosphere, and introducing CO instead2After 1h of gas activation, at N2Cooling to room temperature under atmosphere to obtain CO2Activating the biochar catalyst. The invention greatly reduces the oxygen content on the surface of the carbon material through high-temperature activation, and improves the reducibility of the carbon material. Meanwhile, the carbon material begins to generate a graphitization process through high-temperature treatment, the electron transmission capability of the material is greatly improved, and the material is used as an electron transmission medium to promote the electron transmission degradation process of the phenolic pollutant-persulfate. The invention has the characteristics of cheap and easily obtained catalyst raw materials, simple preparation, high reaction rate, no secondary pollution such as metal leaching and the like.

Description

By using CO2Method for removing phenols in water by activated charcoal activated persulfate degradation
Technical Field
The invention belongs to the technical field of water treatment, and particularly relates to a method for utilizing CO2A method for removing phenols in water by activated charcoal to activate persulfate for degradation.
Background
Phenolic compounds are common organic pollutants in water, the total number of the phenolic compounds is hundreds, the sources of the phenolic compounds are wide, and industrial emission, pesticide degradation and biogeochemical circulation of the environment such as coking, papermaking, medicines, printing and dyeing, chemical engineering and the like can be generated.
The persulfate-based advanced oxidation method is a fenton-like advanced oxidation method emerging in recent years. Compared with hydrogen peroxide, the persulfate is solid at normal temperature, and is easy to store and transport; the cost is lower ($0.74/kg vs $ 1.5/kg); the persulfate radical oxidation potential is higher than the hydroxyl radical OH oxidation potential (3.1V vs2.8V); the persulfate activation method is more various. Accordingly, the persulfate-based advanced oxidation technology has received extensive attention from researchers in recent years.
There are three main methods of persulfate activation: activation by external energy (ultrasound, heat or ultraviolet); transition metal (Fe, Co, Mn) based homogeneous, heterogeneous catalysts; metal free carbon based catalysts. But the added energy activation greatly reduces the economy and limits the large-scale use; the transition metal-based catalyst is difficult to completely solve the problem of dissolution of toxic metal ions. In order to overcome the problems, the metal-free carbon-based catalyst has attracted much attention in recent years, mainly based on nano carbon materials such as graphene oxide, carbon nano tubes, carbon nano-diamond, ordered mesoporous carbon and the like, but research on efficient catalysis of persulfate on degradation of organic pollutants by low-cost biomass-based porous carbon materials has been reported only rarely.
Disclosure of Invention
The technical problem to be solved by the invention is to overcome the defects in the prior art and provide a method for utilizing CO2A method for removing phenols in water by activated charcoal to activate persulfate for degradation.
In order to solve the technical problem, the solution of the invention is as follows:
firstly, providing a CO2The preparation method of the activated charcoal catalyst comprises the following steps:
(1) placing microcrystalline cellulose in a tube furnace in N2Heating to 500 ℃ in the atmosphere, and carbonizing for 3 hours to obtain unactivated biochar;
(2) continue at N2Raising the temperature to 800-950 ℃ in the atmosphere, and introducing CO instead2A gas; after keeping the temperature condition for activation for 1h, in N2Cooling to room temperature under atmosphere to obtain CO2Activating the biochar catalyst.
In the invention, the heating rate is 10 ℃/min.
In the invention, CO is introduced in the step (2)2The flow rate of the gas was controlled to 500 mL/min.
The invention further provides CO prepared by the method2The activated charcoal catalyst is activatedThe method for removing phenols in water by sulfate degradation comprises the steps of placing a container containing waste water on a shaking table, adding the catalyst and persulfate into the waste water, and removing phenol pollutants in the waste water through oxidation reaction; in the process, the reaction conditions are controlled as follows: normal pressure and reaction temperature of 25-45 ℃; the pH value of the initial wastewater is 2.91-9.21; the dosage of the catalyst in the reaction system is 0.1-0.4 g/L, and the concentration of the persulfate is 1-5 mM.
In the invention, the rotating speed of the shaking table is controlled to be 200r/min during the reaction.
Description of the inventive principles:
the invention firstly provides a high-activity metal-free catalyst which is used in persulfate oxidation reaction and can treat phenolic pollutants difficult to degrade. The catalyst takes microcrystalline cellulose biomass as a raw material, biomass-based porous carbon is prepared by a two-step method of carbonization treatment and carbon dioxide activation, and phenolic organic wastewater can be treated under a persulfate oxidation reaction system.
Compared with the prior art, the invention has the beneficial effects that:
(1) the invention passes high-temperature CO2The activation improves the specific surface area of the biochar, enlarges the pore volume, can enhance the adsorption of organic pollutants when used for oxidation reaction, and simultaneously exposes more active sites.
(2) The ratio of C ═ O active sites on the surface of the activated carbon material is increased in the oxygen-containing functional groups, so that the activated persulfate is favorably activated to generate active particle singlet oxygen.
(3) The invention greatly reduces the oxygen content on the surface of the carbon material through high-temperature activation, and improves the reducibility of the carbon material. Meanwhile, the carbon material begins to generate a graphitization process through high-temperature treatment, the electron transmission capability of the material is greatly improved, and the material is used as an electron transmission medium to promote the electron transmission degradation process of the phenolic pollutant-persulfate.
(4) The invention has the characteristics of cheap and easily obtained catalyst raw materials, simple preparation, high reaction rate, no secondary pollution such as metal leaching and the like, and is beneficial to the popularization of the persulfate advanced oxidation technology in the industrial application of the phenol wastewater.
Drawings
FIG. 1 is a graph showing the time-dependent change of the phenol concentration of target pollutants in examples 1-4 in a biomass porous carbon-persulfate system at different activation temperatures.
FIG. 2 is a graph showing the time-dependent change of the concentrations of different phenolic pollutants in examples 5-7 in a 950 ℃ biomass porous carbon-persulfate system.
FIG. 3 is a graph showing the time-dependent change of the concentration of the target pollutant in the biomass porous carbon-persulfate systems (different concentrations) at 950 ℃ in examples 8-9.
FIG. 4 is a graph showing the time-dependent change of the target pollutant concentration in the biomass porous carbon application amount-persulfate system at different temperatures of 950 ℃ in examples 10 to 11.
FIG. 5 is a graph showing the time-dependent change of the concentrations of target pollutants in examples 12 to 14 in a 950 ℃ biomass porous carbon-persulfate system at different pH values of a solution.
FIG. 6 is a graph showing the time-dependent change of the concentrations of target pollutants in examples 15 to 16 in a 950 ℃ biomass porous carbon-persulfate system at different solution temperatures.
Detailed Description
For better understanding of the technical solutions of the present invention, the present invention will now be described with reference to the embodiments. In each example, a shaking table is used to keep the reaction system under the condition of rotating and shaking, and the rotating speed of the shaking table is 200 r/min. Meanwhile, phenol (phenol or chlorophenol) model wastewater is adopted, the concentration of the model wastewater is 0.5mM, and the pH value is 2.91-9.21. The microcrystalline cellulose is commercially available, for example, from Henry food Biotech.
Example 1
20g of microcrystalline cellulose are weighed into N2Carbonizing at 500 ℃ for 3h under the atmosphere, and controlling the heating rate to be 10 ℃/min to obtain the original unactivated biochar BC 500. 1g of biochar is placed in a tube furnace, N2Raising the temperature to 950 ℃ under the atmosphere, and introducing CO instead2Activating for 1h, introducing CO2The flow rate of the gas was controlled to 500mL/min (the same in the following examples). Then in N2And cooling to room temperature under the atmosphere to obtain the carbon dioxide activated biochar AC 950.
0.2g/L of AC950 and 5mM of sodium Persulfate (PS) (the concentration here refers to the final concentration of the catalyst and persulfate in the reaction system, and the same is used in the following examples) were placed in an aqueous solution of 0.5mM of phenol-simulated pollutant with pH 7, and the degradation efficiency reached 99% or more under shaking conditions of 200r/min at normal pressure and 25 ℃ for 60 min.
Example 2
20g of microcrystalline cellulose are weighed into N2Carbonizing at 500 ℃ for 3h under the atmosphere, and controlling the heating rate to be 10 ℃/min to obtain the original biochar BC 500. 1g of biochar is placed in a tube furnace, N2Raising the temperature to 900 ℃ under the atmosphere, and introducing CO instead2Activated for 1h and then at N2And cooling to room temperature under the atmosphere to obtain the carbon dioxide activated charcoal AC 900.
0.2g/L of AC900 and 5mM of sodium Persulfate (PS) are placed in 0.5mM of phenol simulated pollutant aqueous solution with the pH value of 7, and the degradation efficiency reaches over 85 percent within 60min under the conditions of 200r/min shaking and normal pressure and the temperature of 25 ℃.
Example 3
20g of microcrystalline cellulose are weighed into N2Carbonizing at 500 ℃ for 3h under the atmosphere, and controlling the heating rate to be 10 ℃/min to obtain the original biochar BC 500. 1g of biochar is placed in a tube furnace, N2Raising the temperature to 850 ℃ under the atmosphere, and introducing CO instead2Activated for 1h and then at N2And cooling to room temperature under the atmosphere to obtain the carbon dioxide activated charcoal AC 850.
0.2g/L of AC850 and 5mM of sodium Persulfate (PS) are placed in 0.5mM of phenol simulated pollutant aqueous solution with the pH value of 7, and the degradation efficiency reaches over 51 percent within 60min under the conditions of 200r/min shaking and normal pressure and the temperature of 25 ℃.
Example 4
20g of microcrystalline cellulose are weighed into N2Carbonizing at 500 ℃ for 3h under the atmosphere, and controlling the heating rate to be 10 ℃/min to obtain the original biochar BC 500. 1g of biochar is placed in a tube furnace, N2Raising the temperature to 800 ℃ under the atmosphere, and introducing CO instead2Activated for 1h and then at N2And cooling to room temperature under the atmosphere to obtain the carbon dioxide activated biochar AC 800.
0.2g/L of AC800 and 5mM of sodium Persulfate (PS) are placed in 0.5mM of phenol simulated pollutant aqueous solution with the pH value of 7, and the degradation efficiency reaches over 27 percent within 60min under the conditions of 200r/min shaking and normal pressure and the temperature of 25 ℃.
Example 5
20g of microcrystalline cellulose are weighed into N2Carbonizing at 500 ℃ for 3h under the atmosphere, and controlling the heating rate to be 10 ℃/min to obtain the original biochar BC 500. 1g of biochar is placed in a tube furnace, N2Raising the temperature to 950 ℃ under the atmosphere, and introducing CO instead2Activated for 1h and then at N2And cooling to room temperature under the atmosphere to obtain the carbon dioxide activated biochar AC 950.
0.2g/L of AC950 and 5mM of sodium Persulfate (PS) are placed in an aqueous solution of 0.5mM of monochlorophenol simulated pollutant with the pH value of 7, and the degradation efficiency reaches over 99 percent within 60min under the conditions of 200r/min shaking and normal pressure and 25 ℃.
Example 6
20g of microcrystalline cellulose are weighed into N2Carbonizing at 500 ℃ for 3h under the atmosphere, and controlling the heating rate to be 10 ℃/min to obtain the original biochar BC 500. 1g of biochar is placed in a tube furnace, N2Raising the temperature to 950 ℃ under the atmosphere, and introducing CO instead2Activated for 1h and then at N2And cooling to room temperature under the atmosphere to obtain the carbon dioxide activated biochar AC 950.
0.2g/L of AC950 and 5mM of sodium Persulfate (PS) are placed in an aqueous solution of 0.5mM of dichlorophenol simulated pollutants with the pH value of 7, and the degradation efficiency reaches over 98 percent within 60min under the conditions of 200r/min shaking and normal pressure and the temperature of 25 ℃.
Example 7
20g of microcrystalline cellulose are weighed into N2Carbonizing at 500 ℃ for 3h under the atmosphere, and controlling the heating rate to be 10 ℃/min to obtain the original biochar BC 500. 1g of biochar is placed in a tube furnace, N2Raising the temperature to 950 ℃ under the atmosphere, and introducing CO instead2Activated for 1h and then at N2And cooling to room temperature under the atmosphere to obtain the carbon dioxide activated biochar AC 950.
0.2g/L of AC950 and 5mM of sodium Persulfate (PS) are placed in an aqueous solution of 0.5mM of trichlorophenol simulated pollutants with the pH value of 7, and the degradation efficiency reaches over 97 percent within 60min under the conditions of 200r/min shaking and normal pressure and 25 ℃.
Example 8
20g of microcrystalline cellulose are weighed into N2Carbonizing at 500 ℃ for 3h under the atmosphere, and controlling the heating rate to be 10 ℃/min to obtain the original biochar BC 500. 1g of biochar is placed in a tube furnace, N2Raising the temperature to 950 ℃ under the atmosphere, and introducing CO instead2Activated for 1h and then at N2And cooling to room temperature under the atmosphere to obtain the carbon dioxide activated biochar AC 950.
0.2g/L of AC950 and 1mM of sodium Persulfate (PS) are placed in 0.5mM of phenol simulated pollutant aqueous solution with the pH value of 7, and the degradation efficiency reaches over 88 percent within 60min under the conditions of 200r/min shaking and normal pressure and 25 ℃.
Example 9
20g of microcrystalline cellulose are weighed into N2Carbonizing at 500 ℃ for 3h under the atmosphere, and controlling the heating rate to be 10 ℃/min to obtain the original biochar BC 500. 1g of biochar is placed in a tube furnace, N2Raising the temperature to 950 ℃ under the atmosphere, and introducing CO instead2Activated for 1h and then at N2And cooling to room temperature under the atmosphere to obtain the carbon dioxide activated biochar AC 950.
0.2g/L of AC950 and 2mM of sodium Persulfate (PS) are placed in 0.5mM of phenol simulated pollutant aqueous solution with the pH value of 7, and the degradation efficiency reaches over 97 percent within 60min under the conditions of 200r/min shaking and normal pressure and the temperature of 25 ℃.
Example 10
20g of microcrystalline cellulose are weighed into N2Carbonizing at 500 ℃ for 3h under the atmosphere, and controlling the heating rate to be 10 ℃/min to obtain the original biochar BC 500. 1g of biochar is placed in a tube furnace, N2Raising the temperature to 950 ℃ under the atmosphere, and introducing CO instead2Activated for 1h and then at N2And cooling to room temperature under the atmosphere to obtain the carbon dioxide activated biochar AC 950.
0.1g/L of AC950 and 5mM of sodium Persulfate (PS) are placed in 0.5mM of phenol simulated pollutant aqueous solution with the pH value of 7, and the degradation efficiency reaches more than 89% within 60min under the conditions of 200r/min shaking and normal pressure and 25 ℃.
Example 11
20g of microcrystalline cellulose are weighed into N2Carbonizing at 500 ℃ for 3h under the atmosphere, and controlling the heating rate to be 10 ℃/min to obtain the original biochar BC 500. 1g of biochar is placed in a tube furnace, N2Raising the temperature to 950 ℃ under the atmosphere, and introducing CO instead2Activated for 1h and then at N2And cooling to room temperature under the atmosphere to obtain the carbon dioxide activated biochar AC 950.
0.4g/L of AC950 and 5mM of sodium Persulfate (PS) are placed in 0.5mM of phenol simulated pollutant aqueous solution with the pH value of 7, and the degradation efficiency reaches over 98 percent within 60min under the conditions of 200r/min shaking and normal pressure and the temperature of 25 ℃.
Example 12
20g of microcrystalline cellulose are weighed into N2Carbonizing at 500 ℃ for 3h under the atmosphere, and controlling the heating rate to be 10 ℃/min to obtain the original biochar BC 500. 1g of biochar is placed in a tube furnace, N2Raising the temperature to 950 ℃ under the atmosphere, and introducing CO instead2Activated for 1h and then at N2And cooling to room temperature under the atmosphere to obtain the carbon dioxide activated biochar AC 950.
0.2g/L of AC950 and 5mM of sodium Persulfate (PS) are placed in an aqueous solution of 0.5mM of trichlorophenol simulated pollutants with the pH value of 2.91, and the degradation efficiency reaches over 97 percent within 60min under the conditions of normal pressure and 25 ℃ under the shaking condition of 200 r/min.
Example 13
20g of microcrystalline cellulose are weighed into N2Carbonizing at 500 ℃ for 3h under the atmosphere, and controlling the heating rate to be 10 ℃/min to obtain the original biochar BC 500. 1g of biochar is placed in a tube furnace, N2Raising the temperature to 950 ℃ under the atmosphere, and introducing CO instead2Activated for 1h and then at N2And cooling to room temperature under the atmosphere to obtain the carbon dioxide activated biochar AC 950.
0.2g/L of AC950 and 5mM of sodium Persulfate (PS) are placed in an aqueous solution of 0.5mM of trichlorophenol simulated pollutant with the pH value of 4.86, and the degradation efficiency reaches over 97 percent within 60min under the conditions of 200r/min shaking and normal pressure and the temperature of 25 ℃.
Example 14
20g of microcrystalline cellulose are weighed into N2Carbonizing at 500 ℃ for 3h under the atmosphere, and controlling the heating rate to be 10 ℃/min to obtain the original biochar BC 500. 1g of biochar is placed in a tube furnace, N2Raising the temperature to 950 ℃ under the atmosphere, and introducing CO instead2Activated for 1h and then at N2And cooling to room temperature under the atmosphere to obtain the carbon dioxide activated biochar AC 950.
0.2g/L of AC950 and 5mM of sodium Persulfate (PS) are placed in an aqueous solution of 0.5mM of trichlorophenol simulated pollutants with the pH value of 9.21, and the degradation efficiency reaches over 97 percent within 60min under the conditions of 200r/min shaking and normal pressure and the temperature of 25 ℃.
Example 15
20g of microcrystalline cellulose are weighed into N2Carbonizing at 500 ℃ for 3h under the atmosphere, and controlling the heating rate to be 10 ℃/min to obtain the original biochar BC 500. 1g of biochar is placed in a tube furnace, N2Raising the temperature to 950 ℃ under the atmosphere, and introducing CO instead2Activated for 1h and then at N2And cooling to room temperature under the atmosphere to obtain the carbon dioxide activated biochar AC 950.
0.2g/L of AC950 and 5mM of sodium Persulfate (PS) are placed in an aqueous solution of 0.5mM of trichlorophenol simulated pollutants with the pH value of 7, and the degradation efficiency reaches over 97 percent within 60min under the conditions of 200r/min shaking and normal pressure and the temperature of 35 ℃.
Example 16
20g of microcrystalline cellulose are weighed into N2Carbonizing at 500 ℃ for 3h under the atmosphere, and controlling the heating rate to be 10 ℃/min to obtain the original biochar BC 500. 1g of biochar is placed in a tube furnace, N2Raising the temperature to 950 ℃ under the atmosphere, and introducing CO instead2Activated for 1h and then at N2And cooling to room temperature under the atmosphere to obtain the carbon dioxide activated biochar AC 950.
0.2g/L of AC950 and 5mM of sodium Persulfate (PS) are placed in an aqueous solution of 0.5mM of trichlorophenol simulated pollutants with the pH value of 7, and the degradation efficiency reaches over 97 percent within 60min under the conditions of 200r/min shaking and normal pressure and 45 ℃.
The comparative data of the performance of the carbon dioxide activated charcoal in catalyzing persulfate and other charcoal based catalysts in the invention are shown in the following table:
Figure BDA0002154784970000071
as can be seen from the data in the table, the persulfate activation capacity of the carbon dioxide activated biochar is obviously higher than that of other biomass-based carbon materials, which means that the carbon dioxide activated biochar can be degraded in a shorter time by using a smaller amount of catalyst and a smaller amount of oxidant, and the capacity of the biomass-based carbon material for activating persulfate is obviously improved, so that the possibility of applying the biomass-based carbon material for activating persulfate to degrade pollutants is provided.
The raw material of the catalyst used in the invention is cellulose biomass, so the cost is low; the preparation process is simple, does not relate to corrosive and toxic medicines, and is environment-friendly; the catalyst does not contain metal, so that secondary pollution in the using process is avoided, the activation mechanism is mainly a non-free radical path, the reaction rate is high, and the persulfate oxidant is saved. The activated carbon at 950 ℃ can degrade 0.5mM phenol solution by more than 97% within 60 minutes under the conditions of 0.2g/L of catalyst usage amount and 2mM of persulfate concentration. All the catalysts can be regenerated by a method of treating for 1 hour at 700 ℃ under an inert atmosphere, and the performance of the regenerated catalysts is recovered by more than 94 percent.

Claims (2)

1. By using CO2A method for degrading and removing phenols in water by activating a biological carbon catalyst and activating persulfate is characterized in that a container containing wastewater is placed on a shaking bed, the catalyst and the persulfate are added into the wastewater, and phenol pollutants in the wastewater are removed through an oxidation reaction; in the process, the reaction conditions are controlled as follows: normal pressure and reaction temperature of 25-45 ℃; the pH value of the initial wastewater is 2.91-9.21; the adding amount of the catalyst in the reaction system is 0.1-0.4 g/L, and the concentration of the persulfate is 1-5 mM;
the CO is2The activated charcoal catalyst is prepared by the following method: (1) placing microcrystalline cellulose in a tube furnace in N2Heating to 500 deg.C at a rate of 10 deg.C/min under atmosphere, carbonizing for 3 hrObtaining non-activated charcoal; (2) continue at N2Raising the temperature to 800-950 ℃ at the speed of 10 ℃/min in the atmosphere, and introducing CO instead2The flow rate of the gas is controlled to be 500 mL/min; after keeping the temperature condition for activation for 1h, in N2Cooling to room temperature under atmosphere to obtain CO2Activating the biochar catalyst.
2. The method of claim 1, wherein the shaking table is controlled to rotate at a speed of 200r/min during the reaction.
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