CN111545167B - Method for preparing silver ion selective adsorbent by using pasture - Google Patents

Method for preparing silver ion selective adsorbent by using pasture Download PDF

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CN111545167B
CN111545167B CN202010287648.7A CN202010287648A CN111545167B CN 111545167 B CN111545167 B CN 111545167B CN 202010287648 A CN202010287648 A CN 202010287648A CN 111545167 B CN111545167 B CN 111545167B
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biochar
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silver ion
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CN111545167A (en
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邵鹏辉
姚子威
罗旭彪
裴俊俊
罗嘉鑫
杨利明
石慧
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Nanchang Hangkong University
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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
    • 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
    • C02F2101/00—Nature of the contaminant
    • C02F2101/10—Inorganic compounds
    • C02F2101/20—Heavy metals or heavy metal compounds

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Abstract

A method for preparing a silver ion selective adsorbent by using pasture, and relates to a method for preparing a silver ion selective adsorbent. The invention aims to solve the technical problems that the existing adsorbing material is difficult to selectively adsorb silver ions from a complex environment, and has small adsorption quantity and high manufacturing cost. According to the invention, the mercapto is grafted on the surface of the biochar through dehydration condensation of thioglycolic acid and hydroxyl on the surface of the biochar, the mercapto is selective to silver ions, and the mercapto is grafted on the surface of the biochar to provide more adsorption sites for adsorption of the silver ions, so that the selectivity and the adsorption performance to the silver ions are greatly improved. The sulfhydrylation grass biochar is prepared by taking grass as a precursor, is a cheap silver ion selective adsorbent, has strong silver ion selective adsorption performance, is low in production cost and simple in preparation process, and has a great application prospect in actual wastewater treatment. The invention is applied to adsorbing silver ions.

Description

Method for preparing silver ion selective adsorbent by using pasture
Technical Field
The invention relates to a method for preparing a silver ion selective adsorbent.
Background
The pasture grass has various varieties, wide distribution in China and strong regeneration capacity, can be harvested for many times in a year, is rich in various trace elements and vitamins, and therefore becomes the first choice for raising livestock. Data show that the number of commercial pasture planting enterprises in China is large at present, and the annual production of pasture in China is nearly 20000 ten thousand tons in recent years. The development market of the domestic pasture industry shows a growing trend in recent years, which is very favorable for the pasture recovery in the future.
Silver has good ductility, electrical conductivity, thermal conductivity, photosensitivity and antibacterial property, each of which isA very useful raw material in industry, and thus the demand for silver, which is one of the noble metals, is high. For example, silver and its compounds are commonly used in wastewater treatment, food, beverage, pharmaceutical processing, and as disinfectants. On the other hand, silver ions are of particularly great environmental concern due to their potential impact on human health and ecosystem. It has been reported that when silver ions enter the human body, silver is metabolized and deposited in subcutaneous fat, causing psoriasis, where the affected person causes discoloration of the skin. Furthermore, Na is inhibited by silver ion exposure+And Cl-Uptake thereby leads to dysregulation of ions in the human body. The World Health Organization (WHO) and the united states Environmental Protection Agency (EPA) limit the silver content of drinking water to 100ppb (100 g/L). Therefore, with increasing concerns about the toxicity of soluble silver ions in water and the scarcity of silver, it is highly desirable to remove and recover silver ions from water. However, the existing adsorbing material is difficult to selectively adsorb silver ions from a complex environment, and has small adsorption amount and high manufacturing cost.
Disclosure of Invention
The invention provides a method for preparing a silver ion selective adsorbent by using pasture, aiming at solving the technical problems that the existing adsorbing material is difficult to selectively adsorb silver ions from a complex environment, and has small adsorbing capacity and high manufacturing cost.
The method for preparing the silver ion selective adsorbent by using pasture comprises the following steps:
firstly, placing dried pasture in a plant grinder, grinding for 5-10 min, then passing through a 50-mesh sieve to obtain pasture powder, adding the pasture powder into a reaction kettle, adding deionized water, placing in an oven for hydrothermal carbonization, centrifuging a product after the hydrothermal carbonization by using the deionized water until a supernatant is clear and transparent, and drying a solid obtained by centrifugation to obtain hydrated carbon;
in the hydrothermal carbonization process, the mass ratio of the grass powder to the deionized water is 1 (10-12), the hydrothermal temperature is 220-240 ℃, and the hydrothermal time is 12-14 h;
the centrifugal rotating speed is 10000r/min to 12000r/min, and the centrifugal time is 8min to 10 min;
the drying temperature is 110-120 ℃, and the drying time is 12-14 h;
uniformly mixing the hydrated carbon prepared in the step one with an activating agent, grinding, performing high-temperature pyrolysis under the protection of protective gas, cooling to room temperature along with a furnace under the protection of protective gas to obtain a biochar crude product, performing acid washing in a beaker, washing with water to neutrality, performing suction filtration to obtain a black filter cake, and drying the product to obtain biochar;
the activating agent is KOH;
the mass ratio of the hydrated carbon to the activating agent is 1 (4-5);
under the high-temperature pyrolysis condition: the heating rate is 3 ℃/min to 5 ℃/min, the pyrolysis temperature is 800 ℃ to 1000 ℃, and the pyrolysis time is 2h to 3 h;
the flow rate of the protective gas is 150 mL/min-200 mL/min;
the acid for acid cleaning is hydrochloric acid aqueous solution, and the concentration of the hydrochloric acid aqueous solution is 2-3 mol/L;
the volume ratio of the mass of the activating agent to the hydrochloric acid aqueous solution is 8mg (1 mL-1.2 mL);
the drying temperature is 110-120 ℃, and the drying time is 12-14 h;
thirdly, uniformly mixing the biochar prepared in the second step with thioglycollic acid, placing the mixture in an oven for heating, and naturally cooling to room temperature; the heating temperature of the oven is 80-90 ℃, and the heating time is 8-9 h;
adding deionized water, stirring for 30-35 min, and performing suction filtration;
thirdly, repeating the second step until the filtrate after suction filtration is neutral, and placing the black filter cake obtained by suction filtration in an oven for drying to obtain the sulfhydrylation grass biochar; the temperature during drying is 60-70 ℃, and the time is 12-13 h;
the volume ratio of the mass of the biochar to the deionized water is 1mg (2 mL-3 mL);
the volume ratio of the mass of the biochar to the thioglycolic acid is (12.5 mg-15 mg) to 1 mL.
According to the invention, the mercapto is grafted on the surface of the biochar through dehydration condensation of thioglycolic acid and hydroxyl on the surface of the biochar, the mercapto is selective to silver ions, and the mercapto is grafted on the surface of the biochar to provide more adsorption sites for adsorption of the silver ions, so that the selectivity and the adsorption performance to the silver ions are greatly improved.
The sulfhydrylation grass biochar is prepared by taking grass as a precursor, is a cheap silver ion selective adsorbent, has strong silver ion selective adsorption performance, has the adsorption capacity of silver ions almost 12 times that of palladium ions and cadmium ions, and has low production cost, simple preparation process and great application prospect in actual wastewater treatment.
Drawings
FIG. 1 is an adsorption measurement attempt in test two;
FIG. 2 is a Langmuir adsorption isotherm model fitted curve for run three;
FIG. 3 is a Freundlich adsorption isotherm model fit curve in experiment three;
FIG. 4 is a graph of a pseudo first order kinetic model of experiment four;
FIG. 5 is a graph of a pseudo-secondary kinetic model of experiment four.
Detailed Description
The first embodiment is as follows: the embodiment is a method for preparing a silver ion selective adsorbent by using pasture, which is specifically carried out according to the following steps:
firstly, placing dried pasture in a plant grinder, grinding for 5-10 min, then passing through a 50-mesh sieve to obtain pasture powder, adding the pasture powder into a reaction kettle, adding deionized water, placing in an oven for hydrothermal carbonization, centrifuging a product after the hydrothermal carbonization by using the deionized water until a supernatant is clear and transparent, and drying a solid obtained by centrifugation to obtain hydrated carbon;
in the hydrothermal carbonization process, the mass ratio of the grass powder to the deionized water is 1 (10-12), the hydrothermal temperature is 220-240 ℃, and the hydrothermal time is 12-14 h;
the centrifugal rotating speed is 10000r/min to 12000r/min, and the centrifugal time is 8min to 10 min;
the drying temperature is 110-120 ℃, and the drying time is 12-14 h;
uniformly mixing the hydrated carbon prepared in the step one with an activating agent, grinding, performing high-temperature pyrolysis under the protection of protective gas, cooling to room temperature along with a furnace under the protection of protective gas to obtain a biochar crude product, performing acid washing in a beaker, washing with water to neutrality, performing suction filtration to obtain a black filter cake, and drying the product to obtain biochar;
the activating agent is KOH;
the mass ratio of the hydrated carbon to the activating agent is 1 (4-5);
under the high-temperature pyrolysis condition: the heating rate is 3 ℃/min to 5 ℃/min, the pyrolysis temperature is 800 ℃ to 1000 ℃, and the pyrolysis time is 2h to 3 h;
the flow rate of the protective gas is 150 mL/min-200 mL/min;
the acid for acid cleaning is hydrochloric acid aqueous solution, and the concentration of the hydrochloric acid aqueous solution is 2-3 mol/L;
the volume ratio of the mass of the activating agent to the hydrochloric acid aqueous solution is 8mg (1 mL-1.2 mL);
the drying temperature is 110-120 ℃, and the drying time is 12-14 h;
thirdly, uniformly mixing the biochar prepared in the second step with thioglycollic acid, placing the mixture in an oven for heating, and naturally cooling to room temperature; the heating temperature of the oven is 80-90 ℃, and the heating time is 8-9 h;
adding deionized water, stirring for 30-35 min, and performing suction filtration;
thirdly, repeating the second step until the filtrate after suction filtration is neutral, and placing the black filter cake obtained by suction filtration in an oven for drying to obtain the sulfhydrylation grass biochar; the temperature during drying is 60-70 ℃, and the time is 12-13 h;
the volume ratio of the mass of the biochar to the deionized water is 1mg (2 mL-3 mL);
the volume ratio of the mass of the biochar to the thioglycolic acid is (12.5 mg-15 mg) to 1 mL.
The second embodiment is as follows: the first difference between the present embodiment and the specific embodiment is: the pasture in the step one is stipa capillata pasture, alfalfa, sarsa or Chinese fescue. The rest is the same as the first embodiment.
The third concrete implementation mode: the present embodiment differs from the first or second embodiment in that: and the protective gas in the second step is argon. The others are the same as in the first or second embodiment.
The fourth concrete implementation mode: the difference between this embodiment mode and one of the first to third embodiment modes is: and the mass ratio of the hydrated carbon to the activating agent in the step two is 1: 4. The rest is the same as one of the first to third embodiments.
The fifth concrete implementation mode: the fourth difference between this embodiment and the specific embodiment is that: and (2) under the high-temperature pyrolysis condition in the step two: the heating rate is 3 ℃/min, the pyrolysis temperature is 800 ℃, and the pyrolysis time is 2 h. The rest is the same as the fourth embodiment.
The sixth specific implementation mode: the fourth difference between this embodiment and the specific embodiment is that: the volume ratio of the mass of the biochar to the thioglycolic acid in the third step is 12.5mg to 1 mL. The rest is the same as the fourth embodiment.
The invention was verified with the following tests:
test one: the test is a method for preparing the silver ion selective adsorbent by using pasture, and is specifically carried out according to the following steps:
firstly, placing dried pasture into a plant grinder, grinding for 5min, then sieving with a 50-mesh sieve to obtain pasture powder (the powder can pass through a sieve), adding the pasture powder into a reaction kettle, adding deionized water, placing into an oven for hydrothermal carbonization, centrifuging a product after the hydrothermal carbonization with the deionized water until a supernatant is clear and transparent, and drying a solid obtained by centrifugation to obtain hydrated carbon;
the pasture is stipa capillata pasture;
in the hydrothermal carbonization process, the mass ratio of the pasture grass powder to the deionized water is 1:10, the hydrothermal temperature is 220 ℃, and the hydrothermal time is 12 hours;
the rotating speed of the centrifugation is 10000r/min, and the centrifugation time is 8 min;
the drying temperature is 110 ℃, and the drying time is 12 h;
uniformly mixing the hydrated carbon prepared in the step one with an activating agent, grinding, performing high-temperature pyrolysis under the protection of protective gas, cooling to room temperature along with a furnace under the protection of protective gas to obtain a biochar crude product, performing acid washing in a beaker, washing with water to neutrality, performing suction filtration to obtain a black filter cake, and drying the product to obtain biochar;
the protective gas is argon;
the activating agent is KOH;
the mass ratio of the hydrated carbon to the activating agent is 1: 4;
under the high-temperature pyrolysis condition: the heating rate is 3 ℃/min, the pyrolysis temperature is 800 ℃, and the pyrolysis time is 2 h;
the flow rate of the protective gas is 150 mL/min;
the acid for acid cleaning is hydrochloric acid aqueous solution, and the concentration of the hydrochloric acid aqueous solution is 2 mol/L;
the volume ratio of the mass of the activating agent to the hydrochloric acid aqueous solution is 8mg:1 mL;
the drying temperature is 110 ℃, and the drying time is 12 hours;
thirdly, uniformly mixing the biochar prepared in the second step with thioglycollic acid, placing the mixture in an oven for heating, and naturally cooling to room temperature; the heating temperature of the oven is 80 ℃, and the heating time is 8 h;
adding deionized water, stirring for 30min, and then carrying out suction filtration;
thirdly, repeating the second step until the filtrate after suction filtration is neutral, and placing the black filter cake obtained by suction filtration in an oven for drying to obtain the sulfhydrylation grass biochar; the drying temperature is 60 ℃, and the drying time is 12 hours;
the volume ratio of the mass of the biochar to the deionized water is 1mg:2 mL;
the volume ratio of the mass of the biochar to the thioglycolic acid is 12.5mg to 1 mL.
And (2) test II: the test is an adsorption contrast test of sulfhydrylation biochar on different heavy metal ions, and the specific process is as follows:
selection of Cd2+、Pd2+And Ag+And (3) comparison:
50mL of cadmium nitrate aqueous solution (Cd) is measured respectively2+At a concentration of 300mg/L), an aqueous copper sulfate solution (Pd2+At a concentration of 300mg/L) and an aqueous silver nitrate solution (Ag)+300mg/L) are added into a 250mL conical flask together, the concentration of three ions in the mixed solution is 100mg/L, 15mg of sulfhydrylation biochar prepared in the first test is weighed and added into the conical flask, the sulfhydrylation biochar is uniformly dispersed by ultrasonic treatment for 1min and is put into a shaking table to be oscillated for 20h for adsorption, after the adsorption process is finished, the concentration after adsorption is measured by an atomic spectrophotometer, and the Cd pair is calculated2+、Pd2+、Ag+Adsorption capacity of three metal ions; the shaking table is set at 25 ℃ and the rotating speed is 180 rpm.
FIG. 1 shows the adsorption measurement in test two, curve 1 shows Ag+Curve 2 is Pd2+Curve 3 is Cd2+It can be seen that the adsorption capacity of the sulfhydrylation biochar to silver ions is far greater than that of palladium ions and cadmium ions, the maximum adsorption capacity to the silver ions reaches 773.4mg/g, the maximum adsorption capacity to the palladium ions and the cadmium ions is only 96.74mg/g and 65.25mg/g, and the adsorption capacity to the silver ions is nearly 12 times that of the palladium ions and the cadmium ions, which indicates that the sulfhydrylation biochar prepared in the first test has very excellent selectivity to silver ion adsorption.
And (3) test III: the test is an adsorption isotherm test of silver ions adsorbed by sulfhydrylation biochar, and specifically comprises the following steps:
respectively measuring 8 parts of 50mL silver nitrate aqueous solutions with different silver ion concentrations, respectively adding the silver nitrate aqueous solutions into 100mL conical flasks, respectively measuring 5mg of sulfhydrylation biochar prepared by the test I, adding the sulfhydrylation biochar into the conical flasks, respectively carrying out ultrasonic treatment for 1min to ensure that the sulfhydrylation biochar is uniformly dispersed, respectively placing the sulfhydrylation biochar into a shaking table for oscillation and adsorption, measuring the concentration of adsorbed silver ions by an atomic spectrophotometer after the adsorption process is finished, and calculating the concentration of Ag+The data obtained were fitted to Langmuir and Freundlich isothermal adsorption models.
The concentration of silver ions in the 8 parts of silver nitrate aqueous solution is respectively 30mg/L, 40mg/L, 50mg/L, 60mg/L, 70mg/L, 80mg/L, 90mg/L and 100 mg/L.
FIG. 2 is a Langmuir adsorption isothermal model fitting curve in experiment III, FIG. 3 is a Freundlich adsorption isothermal model fitting curve in experiment III, black points in the curve are actual test data, the curve is a corresponding fitting curve, and R of the curve 220.99011, R of Curve 32At 0.97629, it can be seen that test one prepared thiolated biochar on Ag+The adsorption of (A) is more consistent with Langmuir isothermal adsorption model, which shows that the adsorption sites of the sulfhydrylation biochar are uniform, and the adsorbed silver ions have no transverse interaction.
And (4) testing: the test is an adsorption kinetics test of silver ions adsorbed by sulfhydrylation biochar, and the specific process is as follows:
50mL of silver nitrate aqueous solution in which Ag is contained is measured+Adding the solution to a 100mL conical flask, weighing 5mg of the sulfhydrylated biochar prepared in the first step, adding the weighed sulfhydrylated biochar into the conical flask, performing ultrasonic treatment for 1min to uniformly disperse the sulfhydrylated biochar, placing the mixture into a shaking table to perform oscillation adsorption, sampling according to time in the adsorption process, measuring the concentration of each time point by an atomic spectrophotometer, and calculating the concentration of Ag+Amount of adsorption at each time point.
The sampling time is 1, 3, 5, 7, 10, 15, 20, 30, 60, 120, 180, 240, 300, 360, 420, 480, 600, 720, 840, 960, 1080, 1200, 1320, 1440 and 1740, and the units are minutes.
And performing quasi-first-stage and quasi-second-stage dynamics fitting on the obtained data, wherein FIG. 4 is a pseudo-first-stage dynamics model curve diagram in the fourth experiment, FIG. 5 is a pseudo-second-stage dynamics model curve diagram in the fourth experiment, black points in the diagram are actual test data, and the curves are corresponding fitting curves. Fitting of thiolated biochar to Ag using a quasi-second order kinetic model+The adsorption kinetics experimental data has higher correlation coefficient (R)2>0.99), see Table 1, thus illustrating the test-preparation of thiolated biochar against Ag+The adsorption of (A) is more in line with a pseudo-second order kinetic model. Meanwhile, the obtained sulfhydrylation biochar is calculated for Ag by utilizing a pseudo-second-order kinetic model+Theoretical adsorptionThe amount of 757.57mg/g is nearly the same as the actually measured equilibrium adsorption amount (769.59mg/g), so that the adsorption process can be proved to be more in line with a pseudo-second order kinetic model+The adsorption capacity of (a) is strongly correlated with the adsorption sites on the carbon.
TABLE 1 adsorption model of thiolated biochar
Figure BDA0002449137530000061

Claims (6)

1. A method for preparing a silver ion selective adsorbent by using pasture is characterized by comprising the following steps of:
firstly, placing dried pasture in a plant grinder, grinding for 5-10 min, then passing through a 50-mesh sieve to obtain pasture powder, adding the pasture powder into a reaction kettle, adding deionized water, placing in an oven for hydrothermal carbonization, centrifuging a product after the hydrothermal carbonization by using the deionized water until a supernatant is clear and transparent, and drying a solid obtained by centrifugation to obtain hydrated carbon;
in the hydrothermal carbonization process, the mass ratio of the grass powder to the deionized water is 1 (10-12), the hydrothermal temperature is 220-240 ℃, and the hydrothermal time is 12-14 h;
the centrifugal rotating speed is 10000r/min to 12000r/min, and the centrifugal time is 8min to 10 min;
the drying temperature is 110-120 ℃, and the drying time is 12-14 h;
uniformly mixing the hydrated carbon prepared in the step one with an activating agent, grinding, performing high-temperature pyrolysis under the protection of protective gas, cooling to room temperature along with a furnace under the protection of protective gas to obtain a biochar crude product, performing acid washing in a beaker, washing with water to neutrality, performing suction filtration to obtain a black filter cake, and drying the product to obtain biochar;
the activating agent is KOH;
the mass ratio of the hydrated carbon to the activating agent is 1 (4-5);
under the high-temperature pyrolysis condition: the heating rate is 3 ℃/min to 5 ℃/min, the pyrolysis temperature is 800 ℃ to 1000 ℃, and the pyrolysis time is 2h to 3 h;
the flow rate of the protective gas is 150 mL/min-200 mL/min;
the acid for acid cleaning is hydrochloric acid aqueous solution, and the concentration of the hydrochloric acid aqueous solution is 2-3 mol/L;
the volume ratio of the mass of the activating agent to the hydrochloric acid aqueous solution is 8mg (1 mL-1.2 mL);
the drying temperature is 110-120 ℃, and the drying time is 12-14 h;
thirdly, uniformly mixing the biochar prepared in the second step with thioglycollic acid, placing the mixture in an oven for heating, and naturally cooling to room temperature; the heating temperature of the oven is 80-90 ℃, and the heating time is 8-9 h;
adding deionized water, stirring for 30-35 min, and performing suction filtration;
thirdly, repeating the second step until the filtrate after suction filtration is neutral, and placing the black filter cake obtained by suction filtration in an oven for drying to obtain the sulfhydrylation grass biochar; the temperature during drying is 60-70 ℃, and the time is 12-13 h;
the volume ratio of the mass of the biochar to the deionized water is 1mg (2 mL-3 mL);
the volume ratio of the mass of the biochar to the thioglycolic acid is (12.5 mg-15 mg) to 1 mL.
2. The method for preparing silver ion selective adsorbent using pasture grass according to claim 1, wherein the pasture grass in the first step is Imperata graminis, alfalfa, Shabawa or Festuca sinensis.
3. The method for preparing silver ion selective adsorbent by using pasture grass as claimed in claim 1, characterized in that the shielding gas in step two is argon gas.
4. The method for preparing silver ion selective adsorbent by using pasture grass as claimed in claim 1, wherein the mass ratio of the hydrated carbon to the activating agent in the second step is 1: 4.
5. The method for preparing silver ion selective adsorbent by using pasture grass as claimed in claim 1, characterized in that under the condition of pyrolysis in the second step: the heating rate is 3 ℃/min, the pyrolysis temperature is 800 ℃, and the pyrolysis time is 2 h.
6. The method for preparing silver ion selective adsorbent by using pasture grass as claimed in claim 1, characterized in that the ratio of the mass of biochar to the volume of thioglycolic acid in step three is 12.5mg:1 mL.
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