CN110540261A - Method for adsorbing and degrading PPCPs in water body by using phosphoric acid activated phoenix tree leaf biomass charcoal - Google Patents
Method for adsorbing and degrading PPCPs in water body by using phosphoric acid activated phoenix tree leaf biomass charcoal Download PDFInfo
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- CN110540261A CN110540261A CN201910766829.5A CN201910766829A CN110540261A CN 110540261 A CN110540261 A CN 110540261A CN 201910766829 A CN201910766829 A CN 201910766829A CN 110540261 A CN110540261 A CN 110540261A
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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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—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 surface properties or porosity
- B01J20/28057—Surface area, e.g. B.E.T specific surface area
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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
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Abstract
The invention discloses a method for adsorbing and degrading PPCPs in a water body by using phosphoric acid activated phoenix tree leaf biomass carbon, which comprises the steps of firstly heating and activating phoenix tree leaf and phosphoric acid according to the dipping ratio of 3.0 under the protection of nitrogen to prepare phosphoric acid activated phoenix tree leaf biomass carbon; and then adjusting the pH of the phosphoric acid activated phoenix tree leaf biomass charcoal, adding the phosphoric acid activated phoenix tree leaf biomass charcoal into a water body with PPCPs, and adsorbing the PPCPs at room temperature in a dark condition until the adsorption balance is achieved. The method utilizes garden waste phoenix tree leaf biomass charcoal to adsorb and degrade trace PPCPs in the water body, and the phoenix tree leaf biomass charcoal material has larger specific surface area and pore volume structure which are beneficial to the adsorption of the PPCPs; and the surface of the phoenix tree leaf biomass charcoal contains rich oxygen-containing functional groups, so that the surface of the biomass charcoal has negative charges, has good hydrophilicity and acid-base buffer capacity, and shows good adsorption and fixation effects on PPCPs in a water body.
Description
Technical Field
The invention relates to biomass charcoal, in particular to a method for adsorbing and degrading PPCPs in a water body by using phosphoric acid activated phoenix tree leaf biomass charcoal.
Background
Pharmaceutical and Personal Care Products (PPCPs) are novel environmental pollutants, have strong biological activity and are mostly present in trace concentrations in the environment. PPCPs contamination is of a false persistence, i.e. removal occurs simultaneously with introduction. PPCPs are difficult to degrade and easy to enrich, trace amounts of PPCPs exist in water, and due to the enrichment effect of organisms and the transmission of food chains, the toxicological effect is continuously accumulated, and finally irreversible harm is brought to the ecological environment and human health. Therefore, an environment-friendly material capable of efficiently removing PPCPs in the water body is urgently needed to be found.
The biomass charcoal is a carbonaceous material obtained by pyrolysis of biomass under anaerobic or anoxic conditions, has a good porous structure, a large specific surface area and rich functional groups, and has a good removal effect on PPCPs in a water body.
As a garden waste, the phoenix tree leaf is generally treated by adopting a landfill or incineration method, thereby not only polluting the urban environment, but also achieving the recycling of resources. The biomass charcoal prepared by pyrolyzing the phoenix tree leaves is an important way for realizing resource utilization of garden waste.
The unmodified biomass carbon has limited adsorption capacity on pollutants in water, and the modification treatment can improve the pore structure of the biomass carbon, increase the specific surface area and the number of surface functional groups, improve the adsorption performance and improve the adsorption removal effect on the pollutants in the water.
Disclosure of Invention
The purpose of the invention is as follows: the invention provides a method for adsorbing and degrading PPCPs in a water body by using phosphoric acid activated phoenix tree leaf biomass carbon, which realizes resource utilization of garden waste phoenix tree leaves, and can greatly improve the adsorption performance of PPCPs in the water body by adopting phosphoric acid activation modification.
The technical scheme is as follows:
A method for adsorbing and degrading PPCPs in a water body by using phosphoric acid activated phoenix tree leaf biomass charcoal comprises the following steps:
Heating and activating phoenix tree leaves and phosphoric acid under the protection of nitrogen to obtain phosphoric acid activated phoenix tree leaf biomass charcoal;
And step two, adjusting the pH value of the phosphoric acid activated phoenix tree leaf biomass charcoal to 5.5-6.5, adding the phosphoric acid activated phoenix tree leaf biomass charcoal into a water body with PPCPs, and adsorbing the phosphoric acid activated phoenix tree leaf biomass charcoal under the condition of room temperature and light shielding until the adsorption is balanced.
further, according to the method for adsorbing and degrading PPCPs in the water body by using phosphoric acid activated phoenix tree leaf biomass carbon, the mass ratio of phoenix tree leaves to phosphoric acid in the first step can be 3: 1.
Further, in the method for adsorbing and degrading PPCPs in the water body by using phosphoric acid to activate the phoenix tree leaf biomass carbon, the heating temperature for heating and activating in the first step can be 430-500 ℃.
Further, in the method for adsorbing and degrading PPCPs in the water body by using phosphoric acid activated phoenix tree leaf biomass carbon, pretreatment of drying the phoenix tree leaves at 80-110 ℃ for 20-30h is required before activation in the first step.
Further, the method for adsorbing and degrading PPCPs in the water body by using the phosphoric acid activated phoenix tree leaf biomass charcoal comprises the step of heating and washing the phosphoric acid activated phoenix tree leaf biomass charcoal obtained in the step one for 20-40min by using 0.1-0.2 mol/L hydrochloric acid solution.
Further, in the method for adsorbing and degrading PPCPs in the water body by using phosphoric acid activated phoenix tree leaf biomass charcoal, in the second step, the PPCPs comprise any one of TCS, IBU, NAP or OFL.
the specific surface area of the phosphoric acid activated phoenix tree leaf biomass charcoal obtained by the method reaches more than 489m2/g, and the pore volume reaches 0.62cm 3/g.
Has the advantages that: the invention utilizes phosphoric acid to activate the phoenix tree leaf biomass charcoal to adsorb and degrade four PPCPs, the larger surface area and the rich pore structure of the phoenix tree leaf biomass charcoal material are beneficial to the adsorption of the PPCPs, and the surface of the phoenix tree leaf biomass charcoal contains a large amount of oxygen-containing functional groups, so that the surface of the phoenix tree leaf biomass charcoal has negative charges, has good hydrophilicity and buffering capacity to acid and alkali, and shows good adsorption and fixation effects to the PPCPs in the water body; the invention has simple operation and low investment and operation cost.
Drawings
FIG. 1 is a Zeta potential diagram of the phoenix tree leaf biomass charcoal of example 1;
FIG. 2 is a graph showing the isothermal adsorption of four PPCPs on Firmiana simplex leaf biomass charcoal in example 3.
Detailed Description
Example 1
A method for preparing biomass charcoal by using phosphoric acid to activate phoenix tree leaves comprises the following steps:
(1) weighing phoenix tree leaf with certain mass, drying at 80 deg.C for 30 hr, mixing with pure phosphoric acid at impregnation ratio of 3.0 (mass ratio of pure phosphoric acid to dead leaf is 3:1), and impregnating for 24 hr.
(2) And (2) placing the phoenix tree leaves soaked in the step (1) in a high-temperature tube furnace, activating for 3 hours at 430 ℃ under the protection of nitrogen, cooling to room temperature, and taking out.
(3) and (3) heating and washing the phoenix tree leaf biomass charcoal obtained in the step (2) by using 0.2mol/L hydrochloric acid solution at normal temperature for 20min, reducing the ash content, then washing the biomass charcoal by using distilled water to be neutral, and drying the prepared sample in an oven for 20h to obtain the phoenix tree leaf biomass charcoal.
Example 2
a method for preparing biomass charcoal by using phosphoric acid to activate phoenix tree leaves comprises the following steps:
Step one, preparing phosphoric acid activated phoenix tree leaf biomass charcoal:
(1) Weighing phoenix tree leaves with certain mass, drying at 105 ℃ for 24h, mixing with pure phosphoric acid according to the impregnation ratio of 3.0 (the mass ratio of the pure phosphoric acid to the dead leaves is 3:1), and impregnating for 24 h.
(2) And (2) placing the phoenix tree leaves soaked in the step (1) in a high-temperature tube furnace, activating for 2.5h at 450 ℃ under the protection of nitrogen, cooling to room temperature, and taking out.
(3) And (3) heating and washing the phoenix tree leaf biomass charcoal obtained in the step (2) by using 0.1mol/L hydrochloric acid solution at normal temperature for 30min, reducing the ash content, then washing the biomass charcoal by using distilled water to be neutral, and drying the prepared sample in an oven for 24h to obtain the phoenix tree leaf biomass charcoal.
example 3
A method for preparing biomass charcoal by using phosphoric acid to activate phoenix tree leaves comprises the following steps:
(1) weighing phoenix tree leaf with certain mass, drying at 110 deg.C for 20 hr, mixing with pure phosphoric acid at impregnation ratio of 3.0 (mass ratio of pure phosphoric acid to dead leaf is 3:1), and impregnating for 24 hr.
(2) And (2) placing the phoenix tree leaves soaked in the step (1) in a high-temperature tube furnace, activating for 2 hours at 500 ℃ under the protection of nitrogen, cooling to room temperature, and taking out.
(3) And (3) heating and washing the phoenix tree leaf biomass charcoal obtained in the step (2) by using 0.2mol/L hydrochloric acid solution at normal temperature for 40min, reducing the ash content, then washing the biomass charcoal by using distilled water to be neutral, and drying the prepared sample in an oven for 25h to obtain the phoenix tree leaf biomass charcoal.
example 4
The material characterization procedure for the phosphoric acid activated phoenix tree leaf biomass charcoal in example 2 is as follows:
(1) The surface element composition of the phoenix tree leaf biomass charcoal was determined by X-ray photoelectron spectroscopy (Perkin Elmer PHI 550ESCA/SAM, USA). The Zeta potential was measured using a Zeta potential analyzer (Zeta PALS, Brookhaven, USA).
The method comprises the following specific steps: dispersing 20-40mg phosphoric acid activated phoenix tree leaf biomass charcoal in 1mmol/L sodium chloride solution, dissolving the charcoal better by ultrasonic wave, adjusting the suspension to different pH values, and measuring after 2 days of equilibrium time.
(2) Through the step (1), the composition of the surface elements of the phosphoric acid activated phoenix tree leaf biomass charcoal can be obtained as shown in table 1:
TABLE 1 surface element composition
As can be seen from table 1, the surface elements of the phosphoric acid activated phoenix tree leaf biomass charcoal are mainly C, the content thereof is 88.34%, the O content is 10.65%, which indicates that the surface thereof contains a large amount of oxygen-containing functional groups, and in addition, contains a small amount of N and P.
(3) Through the step (1), a Zeta potential diagram of the phosphoric acid activated biomass charcoal can be obtained, as shown in fig. 1.
As can be seen from fig. 1, the phosphoric phoenix tree leaf biomass charcoal always maintains a negative Zeta potential with the continuous change of pH, which indicates that the phoenix tree leaf biomass charcoal is easier to adsorb positive organic matters. As can be seen from FIG. 1, the Zeta potential value of the phoenix tree leaf biomass charcoal varies with the pH. When the pH value is in the range of 3 to 6, the Zeta potential of the phoenix tree leaf biomass charcoal is gradually reduced, which shows that the negative charge of the biomass charcoal is gradually increased; when the pH value is in the range of 6 to 7, the Zeta potential of the phoenix tree leaf biomass charcoal is gradually increased, which shows that the negative charge of the biomass charcoal is gradually reduced; when the pH is in the range of 7 to 10.5, the Zeta potential of the phoenix tree leaf biomass charcoal is gradually reduced, which shows that the negative charge is gradually increased. Therefore, it is presumed that the biomass charcoal of phoenix tree leaf contains-COOH or-OH on the surface.
(4) The adsorption/desorption isotherm of phosphoric acid-activated phoenix tree leaf biomass charcoal on nitrogen was determined using a specific surface area and pore size distribution determinator (Micrometrics ASAP 2020, micritetics Instrument Co, Norcross, GA) at-196 ℃. The sample is degassed at 105 deg.C for more than 16 hr. The specific surface area is calculated by using a Brunauer-Emmett-Teller (BET) method, and the pore size distribution and the pore volume are calculated by using a Barrett-Joyner-Halenda (BJH) method through a desorption isotherm.
(5) Through the step (4), the specific surface area and pore volume parameters of the phosphoric acid activated phoenix tree leaf biomass charcoal can be obtained as shown in table 2:
TABLE 2 specific surface area and pore volume parameters
b calculated by the Brunauer-Emmett-Teller (BET) method
c micropore volume, calculated by the Horvath-Kawazo method
d mesopore volume, calculated from Vt-Vmicro
e total volume, from P/P0-0.99
As can be seen from Table 2, the phosphoric acid activated phoenix tree leaf biomass charcoal has a large specific surface area of 489m 2/g; has rich pore channels, and simultaneously has mesopore and micropore structures, the total pore volume is 0.62cm3/g, wherein the micropore (0-2nm) volume is 0.33cm3/g, and the mesopore (2-50nm) volume is 0.29cm 3/g. The specific surface area and the pore volume are important factors influencing the adsorption performance, and the phoenix tree leaf biomass charcoal has larger specific surface area and pore volume, so that the charcoal shows excellent adsorption performance on macromolecular substances and small molecular substances.
Example 5
The isothermal adsorption experiment of phosphoric acid activated phoenix tree leaf biomass charcoal on four PPCPs in water comprises the following steps:
(1) Four PPCPs were pre-tested for adsorption at room temperature using the phosphoric acid activated phoenix tree leaf biomass charcoal prepared in example 2. The experiment was performed in EPA sample bottles (25mL), the cap of which was a hollow polyethylene screw cap, and the inner layer of the gasket, which contained a thin layer of polytetrafluoroethylene (Teflon), was chemically inert.
(2) In the adsorption pre-experiment aiming at the four PPCPs in the step (1), each experiment is respectively provided with 6 concentration gradients, and each concentration point is provided with 2 parallel samples so as to reduce accidental errors.
(3) Selecting the phoenix tree leaf biomass charcoal with the optimal adsorption rate range according to the result of the preliminary experiment obtained in the step (2).
(4) And (4) weighing 5-10mg of the phoenix tree leaf biomass charcoal with the optimal adsorption rate range in the step (3) by using balance, placing the phoenix tree leaf biomass charcoal into an EPA sample bottle (25ml), and weighing the mass of the sample bottle before and after the biomass charcoal is added so as to verify whether the weighing is accurate (the error allowable range is +/-0.5 mg).
(5) Adding the prepared 0.02mol/L sodium chloride solution into the phoenix tree leaf biomass charcoal in the step (4) at normal temperature, soaking for 12h, and adjusting the pH value to 6.0 by using 0.1mol/L HCl solution or 0.1mol/L NaOH solution.
(6) And (3) adding methanol stock solutions of TCS, IBU and NAP and an aqueous solution of OFL into the mixed solution in the step (5) by using a micro-syringe at normal temperature, and dropwise adding a sodium chloride solution by using a rubber head dropper until the mixed solution is fully filled, wherein the volume of the stock solution prepared from methanol is less than 0.1 percent of the total volume in order to avoid a cosolvent effect.
(7) Weighing the total weight of the EPA sample bottle in the step (6) at normal temperature to accurately calculate the volume of the sodium chloride solution.
(8) and (4) packaging the EPA sample bottle in the step (7) with aluminum foil at room temperature, and carrying out light-proof treatment.
(9) Rotating the EPA sample bottle in the step (8) on a rotary mixer at the speed of 6r/min for two days at room temperature to ensure that the EPA sample bottle is fully mixed to reach the adsorption equilibrium.
(10) And (4) at room temperature, after the equilibration time is two days, taking off the EPA sample bottle in the step (9), and standing for 12 hours.
(11) centrifuging the EPA sample bottle in the step (10) at the rotating speed of 3500r/min at room temperature, taking the supernatant (if the experiment cannot be immediately carried out, the EPA sample bottle needs to be stored in a refrigerator), measuring the absorption peak area by using a High Performance Liquid Chromatography (HPLC), and analyzing the liquid phase equilibrium concentration of the compound obtained after adsorption.
example 6
The method for adsorbing and degrading PPCPs in the water body by phosphoric acid activated phoenix tree leaf biomass carbon comprises the following steps:
(1) According to the peak area measured by High Performance Liquid Chromatography (HPLC) obtained in example 4 and the corresponding sample loading concentration of PPCPs, a Fruendlich isothermal adsorption model is selected for fitting, and a standard curve is drawn, so that the liquid phase concentration of the PPCPs after adsorption can be obtained, as shown in FIG. 2.
As can be seen from figure 2, when the adsorption equilibrium is reached, the liquid phase concentration range of the adsorbate is 10 < -4 > -101mmol/L, and the solid phase concentration is 10 < -4 > -102mmol/kg, which indicates that the phosphoric acid activated phoenix tree leaf biomass charcoal has better adsorption performance for four PPCPs in water. When the adsorption equilibrium state is reached, the adsorption capacity of the phosphoric acid activated phoenix tree leaf biomass charcoal on 4 PPCPs is different, and the liquid phase concentration increases along with the increase of the solid phase concentration during equilibrium. The order of the adsorption efficiency of the phoenix tree leaf biomass charcoal on the 4 PPCPs is as follows: TCS (triclosan) > OFL (ofloxacin) > NAP (naproxen) > IBU (ibuprofen).
Claims (6)
1. A method for adsorbing and degrading PPCPs in a water body by using phosphoric acid activated phoenix tree leaf biomass charcoal is characterized by comprising the following steps:
Heating and activating phoenix tree leaves and phosphoric acid under the protection of nitrogen to obtain phosphoric acid activated phoenix tree leaf biomass charcoal;
And step two, adjusting the pH value of the phosphoric acid activated phoenix tree leaf biomass charcoal to 5.5-6.5, adding the phosphoric acid activated phoenix tree leaf biomass charcoal into a water body with PPCPs, and adsorbing the phosphoric acid activated phoenix tree leaf biomass charcoal under the condition of room temperature and light shielding until the adsorption is balanced.
2. The method for adsorbing and degrading PPCPs in water by using phosphoric acid activated phoenix tree leaf biomass charcoal as claimed in claim 1, wherein the mass ratio of phoenix tree leaf to phosphoric acid in step one is 3: 1.
3. The method for adsorbing and degrading PPCPs in water body by using phosphoric acid activated phoenix tree leaf biomass charcoal as claimed in claim 1, wherein the heating temperature for heating and activating in the step one is 430-500 ℃.
4. The method for adsorbing and degrading PPCPs in water by using phosphoric acid activated phoenix tree leaf biomass charcoal as claimed in claim 1, wherein pretreatment of drying at 80-110 ℃ for 20-30h is required before phoenix tree leaf activation in step one.
5. The method for adsorbing and degrading PPCPs in water body by using phosphoric acid activated phoenix tree leaf biomass charcoal as claimed in claim 1, wherein the phosphoric acid activated phoenix tree leaf biomass charcoal obtained in step one is heated and washed with 0.1-0.2 mol/L hydrochloric acid solution for 20-40 min.
6. The method for adsorbing and degrading PPCPs in water body by using phosphoric acid activated phoenix tree leaf biomass charcoal as claimed in claim 1, wherein the PPCPs in step two comprises any one of TCS, IBU, NAP or OFL.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112221466A (en) * | 2020-09-30 | 2021-01-15 | 中国地质大学（北京） | Phosphate-iron oxide modified biochar composite material, and preparation method and application thereof |
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| CN105836745A (en) * | 2016-04-01 | 2016-08-10 | 山东建筑大学 | Method for preparing carbon material from phoenix tree leaves |
| CN108217647A (en) * | 2018-01-26 | 2018-06-29 | 上海理工大学 | A kind of wormwood based biomass activated carbon and preparation method thereof and its application |
| CN109796058A (en) * | 2019-01-03 | 2019-05-24 | 华中科技大学 | A method of Cr VI and organic pollutant combined pollution are administered using charcoal |
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| KR20160054938A (en) * | 2014-11-07 | 2016-05-17 | 울산대학교 산학협력단 | Chicken manure biochar activated by phosphoric acid and method for removing lead using the same |
| CN105836745A (en) * | 2016-04-01 | 2016-08-10 | 山东建筑大学 | Method for preparing carbon material from phoenix tree leaves |
| CN108217647A (en) * | 2018-01-26 | 2018-06-29 | 上海理工大学 | A kind of wormwood based biomass activated carbon and preparation method thereof and its application |
| CN109796058A (en) * | 2019-01-03 | 2019-05-24 | 华中科技大学 | A method of Cr VI and organic pollutant combined pollution are administered using charcoal |
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Application publication date: 20191206 |