CN113908810A - Biochar immobilized ionic liquid adsorption material and preparation method and application thereof - Google Patents
Biochar immobilized ionic liquid adsorption material and preparation method and application thereof Download PDFInfo
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Images
Classifications
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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
-
- 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
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
-
- 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
-
- 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
- C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
-
- 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
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
- B01J2220/485—Plants or land vegetals, e.g. cereals, wheat, corn, rice, sphagnum, peat moss
-
- 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
Abstract
The invention discloses a biochar immobilized ionic liquid adsorption material, and a preparation method and application thereof, and belongs to the field of sewage treatment. Raw materials of the adsorbing material comprise peanut shell biochar and ionic liquid, wherein the mass ratio of the peanut shell biochar to the ionic liquid is 1: 0.5-2; the ionic liquid is quaternary ammonium salt ionic liquid or quaternary phosphonium salt ionic liquid. According to the invention, the peanut shell biochar is modified by the ionic liquid to obtain the biochar immobilized ionic liquid adsorbing material, the adsorbing material has high thermal stability and good chemical stability, the required amount of the ionic liquid is small, secondary environmental pollution is avoided, the problem of poor adsorption effect of biochar on anionic heavy metals is solved, and the defects of large amount of the ionic liquid and difficult recovery in the using process are overcome.
Description
Technical Field
The invention relates to a biochar immobilized ionic liquid adsorption material, and a preparation method and application thereof, and belongs to the field of sewage treatment.
Background
With the further development of the national industrialization process and the further increase of the industrial application, the industrial wastewater becomes the largest 'pain point' of the industrial civilization. The pollution problem of heavy metals (such as lead, chromium, mercury, cadmium and the like) in industrial wastewater is particularly serious, and the pollutants cannot be removed by a biodegradation way like organic matters, can be accumulated in organism tissues of organisms, and can cause serious harm to human health and social safety along with the further enrichment of food chain transmission. Chromium (Cr), molybdenum (Mo), vanadium (V) and tungsten (W) have all been used in industrial production, and their electroplating, printing, ore mining, smelting and industrial application may cause environmental pollution problems, and an effective treatment method is urgently needed. Since Cr (VI) has serious harm to animals, plants and human bodies, Cr (VI) is always a pollutant which is preferably controlled by various countries.
The ionic liquid has more special physical and chemical properties, including higher thermal stability, good chemical stability, non-flammability, difficult volatility (negligible vapor pressure), higher viscosity, higher conductivity and wider electrochemical window, good dissolution property, excellent catalytic property, and the like. Compared with the high toxicity, high volatility and inflammability of the traditional organic solvent, the ionic liquid has great advantages. As a green solvent and a novel reaction medium, the ionic liquid is widely applied to the fields of organic synthesis, chemical catalysis, separation and extraction, electrochemistry and the like. However, ionic liquids still have some drawbacks in the above applications: (1) the ionic liquid has a large demand for dosage when used as an extraction solvent and a reaction medium, and the synthesis process of the ionic liquid is complex and therefore the cost is high. (2) The ionic liquid has high viscosity, which is not beneficial to the mass transfer and heat transfer processes. (3) The separation process after extraction is complicated, and the ionic liquid is easy to run off, possibly causing new pollution.
The above drawbacks limit the large-scale application of ionic liquids in industrial production. The problem can be solved well by loading the ionic liquid on some solid materials with excellent physicochemical properties to prepare the 'Supported ionic liquid phase' (SILP). Commonly used solid support materials include activated carbon, silica gel, cellulose, nano metal oxides, and the like.
Biochar (biochar) is a solid material formed from biomass-rich raw material by pyrolysis, carbonization under anaerobic or anaerobic conditions. Various industrial and agricultural wastes in social production, such as fly ash, crop straws, fruit shells, fruit peels, livestock and poultry excrement, sludge in sewage plants and the like, can be used as raw materials for preparing the biochar. The biochar prepared by pyrolysis has the advantages of high carbonization degree, stable chemical property, rich pore structure, large specific surface area and rich surface functional groups. However, the adsorption sites of the biochar to anionic heavy metals are limited, and the ideal removal effect is difficult to achieve.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a biochar immobilized ionic liquid adsorption material, a preparation method and application thereof, so as to solve the problems of poor adsorption effect and high cost of biochar on anionic heavy metals.
In order to achieve the purpose, the invention adopts the technical scheme that: a biochar immobilized ionic liquid adsorption material comprises raw materials of peanut shell biochar and ionic liquid, wherein the mass ratio of the peanut shell biochar to the ionic liquid is 1: 0.5-2; the ionic liquid is quaternary ammonium salt ionic liquid or quaternary phosphonium salt ionic liquid.
According to the invention, the peanut shell biochar is modified by the ionic liquid to obtain the biochar immobilized ionic liquid adsorbing material, and the adsorbing material has high thermal stability and good chemical stability, requires a small amount of the ionic liquid, and cannot cause secondary environmental pollution. Quaternary ammonium salt ions or quaternary phosphonium salt ions on the biochar immobilized ionic liquid adsorption material can be combined with heavy metal ions with negative charges through electrostatic attraction to form compounds with corresponding ion pair forms, so that the adsorption performance of the adsorption material is improved, the problem that the biochar has poor adsorption effect on anionic heavy metal is successfully solved, and the defects that the ionic liquid is large in dosage and difficult to recycle in the use process are overcome.
When the mass ratio of the peanut shell biochar to the ionic liquid is 1:0.5-2, the peanut shell biochar can be fully contacted with the ionic liquid during reaction, the ionic liquid is uniformly distributed on the peanut shell biochar, the content of the ionic liquid is too small to achieve the dispersion effect, the ionic liquid cannot be fully distributed on the peanut shell biochar, and the performance of the adsorbing material cannot be improved; the content of the ionic liquid is too high, the loading capacity of the ionic liquid cannot be obviously increased, and meanwhile, the waste of raw materials is caused, and the economic benefit is influenced.
The quaternary ammonium salt ionic liquid is methyl trioctyl ammonium chloride; the quaternary phosphonium salt ionic liquid is trihexyltetradecyl phosphonium chloride.
As a preferred embodiment of the biochar immobilized ionic liquid adsorption material, the preparation method of the peanut shell biochar comprises the following steps:
(1) cleaning peanut shells, drying, crushing and sieving to obtain peanut shell powder;
(2) and calcining the peanut shell powder, and then washing, filtering and drying the calcined peanut shell powder to obtain the peanut shell biochar.
The purpose of washing the peanut shells is to remove impurities such as soil and dust remaining on the surfaces of the peanut shells.
As a preferred embodiment of the biochar-supported ionic liquid adsorption material, the calcining conditions in the step (2) are as follows: the calcination temperature is 350-500 ℃, the calcination time is 2-4h, and the heating rate is 3-10 ℃/min.
The inventor finds that the peanut shell biochar can form a stable structure at the calcining temperature of 350-500 ℃, and the peanut shell biochar has high crystallinity and complete crystal form. The adverse effects caused by too high a calcination temperature are: the structure of the peanut shell powder is destroyed due to pyrolysis, and the pyrolysis may cause the layered structure of the peanut shell powder to be further peeled off, so that the thickness of the peanut shell biochar is reduced, the surface is roughened, and the stability is reduced. If the calcination temperature is too low, the crystallinity of the peanut shell biochar is poor, the carbonization degree is low, and a pore structure cannot be formed.
In addition, the temperature rise rate can also influence the performance of the adsorbing material, and when the temperature rise rate is 3-10 ℃/min, the adsorbing material can form a mesoporous structure and has high crystallinity. When the temperature rise rate is too high, the peanut shell powder is cracked too fast, the weight loss is too large, the reaction is violent, and the loss is large; the adverse effects of too little temperature rise rate are: the peanut shell powder stays in the temperature range for a long time, the degree difference of the cracking reaction is small, the generation of rich mesoporous structures is not facilitated, and the crystallinity of the material is influenced.
As a preferred embodiment of the biochar-supported ionic liquid adsorbent, the washing method in the step (2) comprises: adding the calcined peanut shell powder into absolute ethyl alcohol, and stirring for 2-4 h; wherein the ratio of the mass of the calcined peanut shell powder to the volume of the absolute ethyl alcohol is 1: 5-15.
The purpose of washing is to remove ash in the peanut shell biochar, wherein the ash is derived from soluble metal salt.
As a preferred embodiment of the biochar-supported ionic liquid adsorption material, the drying temperature of the step (1) is 55-65 ℃.
The inventor finds that when the drying temperature is 55-65 ℃, the surface property of the material cannot be influenced, and the surface moisture of the peanut shell powder can be quickly evaporated and hardened due to overhigh temperature, while the internal moisture is difficult to diffuse out again, so that the structure of the peanut shell powder is influenced; if the temperature is too low, the peanut shell powder may be dried for too long, and the surface of the peanut shell powder may change.
In a second aspect, the invention provides a preparation method of a biochar immobilized ionic liquid adsorption material, which comprises the following steps:
(1) adding ionic liquid into an organic solvent, and stirring and mixing uniformly to obtain a mixed solution;
(2) adding the mixed solution into the peanut shell biochar, stirring and mixing uniformly, then carrying out ultrasonic treatment, filtering, washing and filtering again, and drying the obtained filter medium to obtain the biochar immobilized ionic liquid adsorbing material.
Preferably, the organic solvent is one of methanol, ethanol and acetone.
As an alternative embodiment, the organic solvent is methanol, ethanol or acetone, and it should be noted that the above list of organic solvents is only used to illustrate that the present invention can be implemented, and is not limited to the present invention, and in other embodiments, other solvents can be used by those skilled in the art. Preferably, the organic solvent is acetone.
Preferably, the time of the ultrasound is 0.5 to 1.5 hours.
The dispersibility of ionic liquid can be improved by ultrasound, the removal capacity of heavy metals of the biological carbon immobilized ionic liquid adsorption material is further improved by the aid of physical adsorption of the peanut shell biochar, active components cannot be uniformly dispersed in a pore channel of the peanut shell biochar due to too short ultrasound time, and the ionic liquid overflows the peanut shell biochar due to too long ultrasound time, so that the stability of the adsorption material is influenced.
Preferably, the drying conditions are: the drying temperature is 55-65 ℃, and the drying time is 8-24 h.
In a third aspect, the invention provides an application of a biochar immobilized ionic liquid adsorption material in sewage treatment.
Compared with the prior art, the invention has the beneficial effects that:
(1) quaternary ammonium salt ions or quaternary phosphonium salt ions on the biochar immobilized ionic liquid adsorption material can be combined with heavy metal ions with negative charges through electrostatic attraction to form compounds with corresponding ion pair forms, so that the adsorption performance of the adsorption material is improved, the problem that the biochar has poor adsorption effect on anionic heavy metal is successfully solved, and the defects that the ionic liquid is large in dosage and difficult to recycle in the use process are overcome.
(2) The biochar immobilized ionic liquid adsorbing material has high thermal stability and good chemical stability, requires less ionic liquid and cannot cause secondary environmental pollution.
(3) The biochar immobilized ionic liquid adsorbing material disclosed by the invention also has a good adsorbing effect in an acidic environment, the resolving raw material is cheap and easy to obtain, the adsorbing material is stable in performance and high in recycling rate, and resolved heavy metal can be recycled, so that the adsorbing material has great advantages and potentials in the field of environment, can be used as an efficient, green and environment-friendly solid adsorbent, is applied to a treatment process for recovering leachate of industrial wastewater, ore mining wastewater and waste denitration catalysts, and has a wide prospect for realizing industrial application.
Drawings
FIG. 1 is a flow chart of a preparation method of a biochar-supported ionic liquid adsorption material of the invention;
FIG. 2 is a diagram showing the adsorption effect of the biochar-supported ionic liquid adsorbent according to the present invention;
FIG. 3 is an SEM image of the biochar-supported ionic liquid adsorbent of the invention;
FIG. 4 is an FTIR chart of the biochar-supported ionic liquid adsorbent material of the present invention;
FIG. 5 is an XPS plot of a biochar-immobilized ionic liquid adsorbent;
fig. 6 is a graph showing the analytical effects of different analytical reagents on a biochar-supported ionic liquid adsorbent.
Detailed Description
To better illustrate the objects, aspects and advantages of the present invention, the present invention will be further described with reference to the following detailed description and accompanying drawings.
Fig. 1 is a flow chart of a preparation method of a biochar-supported ionic liquid adsorption material.
In the following examples, the quaternary ammonium salt ionic liquid is methyl trioctyl ammonium chloride; the quaternary phosphonium salt ionic liquid is trihexyltetradecyl phosphonium chloride.
Example 1
The implementation provides a biochar immobilized ionic liquid adsorption material which comprises raw materials of peanut shell biochar and ionic liquid, wherein the mass ratio of the peanut shell biochar to the ionic liquid is 1: 2; the ionic liquid is quaternary ammonium salt ionic liquid.
The embodiment provides a preparation method of a biochar immobilized ionic liquid adsorption material, which comprises the following steps:
(1) washing peanut shells with tap water and deionized water for several times to remove impurities such as soil, dust and the like remained on the surfaces of the peanut shells, then placing the cleaned peanut shells in a drying oven, and drying for 24 hours at 65 ℃; then crushing the dried peanut shells by using a crusher to obtain crushed peanut shells; finally, sieving the crushed peanut shells with a 80-mesh sieve to obtain peanut shell powder;
(2) calcining the peanut shell powder at the temperature of 500 ℃ for 2h at the heating rate of 3 ℃/min to obtain calcined peanut shell powder; adding the calcined peanut shell powder into absolute ethyl alcohol, and mechanically stirring for 4 hours, wherein the ratio of the mass of the calcined peanut shell powder to the volume of the absolute ethyl alcohol is 1: 15; removing organic impurities on the calcined peanut shell powder, washing the peanut shell powder by deionized water for a plurality of times, filtering, and drying the obtained filter medium in a drying box to obtain the peanut shell biochar;
(3) adding 4 parts by mass of quaternary ammonium salt ionic liquid into 8 parts by volume of acetone, and stirring and mixing uniformly to obtain a mixed solution;
(4) adding the mixed solution into 2 parts by mass of peanut shell biochar, uniformly stirring and mixing, performing ultrasonic treatment for 0.5h, filtering the mixture after the ultrasonic treatment is finished, washing the filter medium with pure water, filtering again, and drying the obtained filter medium at 55 ℃ for 24h to obtain the biological other immobilized ionic liquid adsorption material, which is named as BC-IL 1.
Example 2
The implementation provides a biochar immobilized ionic liquid adsorption material which comprises raw materials of peanut shell biochar and ionic liquid, wherein the mass ratio of the peanut shell biochar to the ionic liquid is 1: 1.5; the ionic liquid is a quaternary phosphonium salt ionic liquid.
The embodiment provides a preparation method of a biochar immobilized ionic liquid adsorption material, which comprises the following steps:
(1) washing the peanut shells with tap water and deionized water for several times to remove impurities such as soil, dust and the like remained on the surfaces of the peanut shells, then placing the cleaned peanut shells in an oven, and drying for 2 days at 60 ℃; then crushing the dried peanut shells by using a crusher to obtain crushed peanut shells; finally, sieving the crushed peanut shells through a 100-mesh sieve to obtain peanut shell powder;
(2) calcining the peanut shell powder at 400 ℃ for 2h at a heating rate of 5 ℃/min to obtain calcined peanut shell powder; adding the calcined peanut shell powder into absolute ethyl alcohol, and mechanically stirring for 3 hours, wherein the ratio of the mass of the calcined peanut shell powder to the volume of the absolute ethyl alcohol is 1: 10; removing organic impurities on the calcined peanut shell powder, washing the peanut shell powder by deionized water for a plurality of times, filtering, and drying the obtained filter medium in a drying box to obtain the peanut shell biochar;
(3) adding 3 parts by mass of quaternary phosphonium salt ionic liquid into 8 parts by volume of acetone, and stirring and mixing uniformly to obtain a mixed solution;
(4) adding the mixed solution into 2 parts by mass of peanut shell biochar, uniformly stirring and mixing, performing ultrasonic treatment for 1h, filtering the mixture after the ultrasonic treatment is finished, washing a filter medium with pure water, filtering again, and drying the obtained filter medium at 60 ℃ for 12h to obtain the biochar immobilized ionic liquid adsorbing material named as BC-IL 2.
Example 3
The implementation provides a biochar immobilized ionic liquid adsorption material which comprises raw materials of peanut shell biochar and ionic liquid, wherein the mass ratio of the peanut shell biochar to the ionic liquid is 1: 0.5; the ionic liquid is a quaternary phosphonium salt ionic liquid.
The embodiment provides a preparation method of a biochar immobilized ionic liquid adsorption material, which comprises the following steps:
(1) washing peanut shells with tap water and deionized water for several times to remove impurities such as soil, dust and the like remained on the surfaces of the peanut shells, then placing the cleaned peanut shells in a drying oven, and drying for 3 days at 55 ℃; then crushing the dried peanut shells by using a crusher to obtain crushed peanut shells; finally, sieving the crushed peanut shells through a 120-mesh sieve to obtain peanut shell powder;
(2) calcining the peanut shell powder at 350 ℃ for 4h at a heating rate of 10 ℃/min to obtain calcined peanut shell powder; adding the calcined peanut shell powder into absolute ethyl alcohol, and mechanically stirring for 2 hours, wherein the ratio of the mass of the calcined peanut shell powder to the volume of the absolute ethyl alcohol is 1: 5; removing organic impurities on the calcined peanut shell powder, washing the peanut shell powder by deionized water for a plurality of times, filtering, and drying the obtained filter medium in a drying box to obtain the peanut shell biochar;
(3) adding 1 part by mass of quaternary phosphonium salt ionic liquid into 8 parts by volume of acetone, and stirring and mixing uniformly to obtain a mixed solution;
(4) adding the mixed solution into 2 parts by mass of peanut shell biochar, uniformly stirring and mixing, performing ultrasonic treatment for 1.5h, filtering the mixture after the ultrasonic treatment is finished, washing a filter medium with pure water, filtering again, and drying the obtained filter medium at 65 ℃ for 8h to obtain the biological other immobilized ionic liquid adsorption material named BC-IL 3.
Comparative example 1
The comparative example provides a preparation method of peanut shell biochar, which comprises the following steps:
(1) washing the peanut shells with tap water and deionized water for several times to remove impurities such as soil, dust and the like remained on the surfaces of the peanut shells, then placing the cleaned peanut shells in an oven, and drying for 2 days at 60 ℃; then crushing the dried peanut shells by using a crusher to obtain crushed peanut shells; finally, sieving the crushed peanut shells through a 100-mesh sieve to obtain peanut shell powder;
(2) calcining the peanut shell powder at 400 ℃ for 2h at a heating rate of 5 ℃/min to obtain calcined peanut shell powder; adding the calcined peanut shell powder into absolute ethyl alcohol, and mechanically stirring for 3 hours, wherein the ratio of the mass of the calcined peanut shell powder to the volume of the absolute ethyl alcohol is 1: 10; removing organic impurities on the calcined peanut shell powder, washing the peanut shell powder by deionized water for a plurality of times, filtering, and drying the obtained filter medium in a drying box to obtain the peanut shell biochar which is named as BC.
Experimental example 1
The experimental example tests the adsorption performance of the biochar immobilized ionic liquid adsorption material.
The test principle is as follows: with heavy metal contaminant K2Cr2O7For the target, the adsorption performance of different adsorption materials on cr (vi) was tested.
The test method comprises the following steps:
accurately weighing potassium dichromate (K) by using an analytical balance2Cr2O7) 2.8269g of solid is dissolved by deionized water and then is added into a volumetric flask with 1000mL to prepare 1000mg/L Cr (VI) stock solution. When carrying out the subsequent batch adsorption experiment, diluting the Cr (VI) stock solution by a certain multiple to prepare Cr (VI) use solution with corresponding concentration, and using 1mol/L H2SO4The pH of the solution was adjusted with 1mol/L KOH solution.
The main experimental procedures for carrying out the batch adsorption experiments were as follows: 0.1g of the adsorbent (BC, BC-IL1, BC-IL2) was added to a 50mL centrifuge tube, and 20mL of Cr (VI) solution was added thereto, followed by placing on an incubator shaker and shaking reaction for a while (shaking speed 160 r/min). After the reaction is finished, taking the supernatant in the centrifuge tube, filtering the supernatant through a 0.45 mu m microporous filter membrane by using an injector, measuring the total Cr concentration in the adsorbed solution by using an Atomic Absorption Spectrophotometry (AAS), and measuring the Cr (VI) concentration in the solution by using a dibenzoyl dihydrazide chromogenic spectrophotometry.
The specific steps for measuring the Cr (VI) concentration by using a spectrophotometry method are as follows: weighing 1g of diphenylcarbazide, dissolving in 50mL of acetone, diluting the volume to 100mL with deionized water, dissolving with ultrasonic assistance, and shaking up to obtain the diphenylcarbazide color developing agent. When the color development reaction was performed, 10mL of the solution to be measured was added to the cuvette, 0.1mL (1+1) of sulfuric acid and 0.1mL (1+1) of phosphoric acid were added, and 0.4mL of a dibenzoyl dihydrazide color-developing reagent was added to the cuvette, and after the color development was performed for 5 to 10 minutes, the absorbance was measured at 540 nm. The results are shown in FIG. 2.
Fig. 2 is a diagram of the adsorption effect of the preparation method of the biochar-supported ionic liquid adsorption material of the invention. As can be seen from FIG. 2, the adsorption amounts of BC-IL1 and BC-IL2 to Cr (VI) are much higher than that of BC, the adsorption rate is faster, and the reaction time for reaching the adsorption equilibrium is shorter. For BC, the Cr concentration decreases rapidly within 4 hours from the beginning of the reaction, and then the Cr concentration curve gradually slows down, and the reaction almost reaches equilibrium within about 24 hours. The reaction rates of BC-IL1 and BC-IL2 are faster, the adsorption amounts of the BC-IL1 and the BC-IL2 at 1h reach 8.76mg/g and 9.94mg/g respectively, and account for 94.88 percent and 96.65 percent of the maximum adsorption amount; the adsorption equilibrium is reached approximately 2h, after which there is no longer any significant reduction in the Cr concentration.
Experimental example 2
The experimental example researches the influence of the mass ratio of the peanut shell biochar to the ionic liquid on the adsorption performance of the biochar immobilized ionic liquid adsorption material, experimental groups 1-4 in the experimental example prepare the biochar immobilized ionic liquid adsorption material according to the preparation method in the example 2, except that the mass ratio of the peanut shell biochar to the ionic liquid is different, the other experimental groups 1-4 are the same, the obtained biochar immobilized ionic liquid adsorption material is used for measuring the loading capacity of the ionic liquid in the adsorption material by using a thermogravimetric analyzer, and the result is shown in table 1.
TABLE 1
As can be seen from table 1, the loading amount of the ionic liquid tends to increase continuously with the addition amount of the ionic liquid, and when the mass ratio of the peanut shell biochar to the ionic liquid is greater than 1:1.5, the loading amount of the ionic liquid does not increase significantly, so that the mass ratio of the peanut shell biochar to the ionic liquid is optimally 1: 1.5.
Experimental example 3
The experimental example researches the influence of ultrasonic time on the adsorption performance of the biochar-supported ionic liquid adsorption material, in the experimental example, test groups 5 to 9 prepare the biochar-supported ionic liquid adsorption material according to the preparation method of the example 2, the test groups 5 to 9 are the same except for different ultrasonic times, the obtained biochar-supported ionic liquid adsorption material is used for measuring the loading capacity of ionic liquid in the adsorption material by a thermogravimetric analyzer, and the results are shown in table 2.
TABLE 2
| Test group 5 | Test group 6 | Test group 7 | |
Test group 9 | |
| Time of ultrasound | 10min | 30min | 1h | 2h | 4h |
| Load amount/(g/g) | 0.0784 | 0.1446 | 0.1918 | 0.2021 | 0.1898 |
As can be seen from Table 2, when the ultrasonic time is longer than 1h, the loading amount of the ionic liquid does not increase significantly with the prolongation of the ultrasonic time, and therefore, the optimal ultrasonic time of the invention is 1 h.
Experimental example 4
The experimental example researches the mechanism of adsorbing and removing heavy metals by the biochar immobilized ionic liquid adsorbing material.
BC-IL1 adsorbing Cr (VI) in the experimental example 1 is dried and named BC-IL 1-Cr;
BC-IL2 adsorbing Cr (VI) in the experimental example 1 is dried and named BC-IL 2-Cr; the BC, BC-IL1, BC-IL1-Cr, BC-IL2, BC-IL2-Cr were then characterized by SEM, FTIR, and the results are shown in FIGS. 3-4.
FIG. 3 is an SEM image of the biochar-immobilized ionic liquid adsorbent, wherein a is BC, b is BC-IL1, c is BC-IL1-Cr, d is BC-IL2, and e is BC-IL 2-Cr. As can be seen from the SEM images, many small particles and lumps appear on the surface of BC-IL1-Cr and BC-IL2-Cr as compared with BC, BC-IL1 and BC-IL 2.
FIG. 4 is an FTIR chart of the biochar-supported ionic liquid adsorbent, wherein (a) is BC, (b) is BC-IL1, (c) is BC-IL1-Cr, (d) is BC-IL2, and (e) is BC-IL 2-Cr. As can be seen from FIG. 4, FTTR patterns of BC-IL1-Cr and BC-IL2-Cr were at 938cm in comparison with BC, BC-IL1, BC-IL2-1And 792cm-1Two new peaks appear at the position, and the generation of Cr can be inhibited.
Drying BC-IL1 adsorbed with Cr (Total) in the experimental example 1, and naming BC-IL1-Cr (T); drying BC-IL2 adsorbed with Cr (Total) in the experimental example 1, and naming BC-IL2-Cr (T); BC-IL1-Cr (T), BC-IL1-Cr (T) were then subjected to XPS characterization, and the results are shown in FIG. 5.
FIG. 5 is an XPS diagram of an ion liquid adsorbing material immobilized on biochar, wherein the diagram (a) is BC-IL1-Cr (T), and the diagram (b) is BC-IL2-Cr (T). As can be seen from FIG. 5, the distinct band that appears at the binding energies of 575-3/2Orbital sum 585-1/2A track. Specifically, the peak components at about 576eV and 586eV can be attributed to Cr (III), while the peaks at 578eV and 588eV can be attributed to Cr (VI). The results show that both Cr (VI) and Cr (III) are distributed on the adsorbent material. In addition, by matching two typesThe peak area of Cr ions was quantified and the Cr (VI) content on the adsorbent was found to be 27.08% for BC-IL1-Cr (T) and 38.90% for BC-IL2-Cr (T). Thus, the adsorption process involves a reduction mechanism, BC-IL1-Cr (T) and BC-IL2-Cr (T) with 72.92% and 61.10% of Cr (VI) being reduced to Cr (III), respectively.
Comparing the analysis effects of different analysis reagents, adding BC-IL1-Cr and BC-IL2-Cr into the analysis reagents respectively, wherein the analysis reagents are NaOH solution, HCl solution, ascorbic acid solution, EDTA solution and Na2SO4The solution, the HCl/ascorbic acid mixed solution, and deionized water were used to test the analytical effect of the analytical reagent, and the test results are shown in fig. 6.
FIG. 6 is a graph showing the effect of different analytical reagents on the adsorption of a biochar-supported ionic liquid, wherein BC-IL1-Cr is shown in FIG. a, and BC-IL2-Cr is shown in FIG. b. As can be seen from FIG. 6, HCl alone has a poor desorption effect on Cr, and Na2SO4When the adsorbent is desorbed with deionized water, the desorption efficiency is close to or slightly lower than that of HCl, the desorption effect of EDTA on Cr is also poor, about 40% of adsorbed Cr can be desorbed by using an ascorbic acid solution, and the best desorption effect is a mixed solution of NaOH solution and HCl/ascorbic acid, so that the adsorption mechanism of BC-IL1 and BC-IL2 on Cr (VI) is mainly a process of electrostatic attraction.
Therefore, the biochar-supported ionic liquid adsorbing material can rapidly and efficiently remove heavy metal pollutants Cr (VI) in water, quaternary ammonium salt ions or quaternary phosphonium salt ions on the biochar-supported ionic liquid adsorbing material can be combined with Cr (VI) with negative electricity through electrostatic attraction to form compounds in corresponding ion pair forms, and the adsorption and removal of Cr (VI) in water are accelerated.
Finally, it should be noted that the above embodiments are intended to illustrate the technical solutions of the present invention and not to limit the scope of the present invention, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications and equivalent substitutions can be made to the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (10)
1. The biochar immobilized ionic liquid adsorption material is characterized in that raw materials comprise peanut shell biochar and ionic liquid, wherein the mass ratio of the peanut shell biochar to the ionic liquid is 1: 0.5-2; the ionic liquid is quaternary ammonium salt ionic liquid or quaternary phosphonium salt ionic liquid.
2. The biochar-supported ionic liquid adsorbing material as claimed in claim 1, wherein the preparation method of the peanut shell biochar comprises the following steps:
(1) cleaning peanut shells, drying, crushing and sieving to obtain peanut shell powder;
(2) and calcining the peanut shell powder, and then washing, filtering and drying the calcined peanut shell powder to obtain the peanut shell biochar.
3. The biochar-supported ionic liquid adsorbing material as claimed in claim 2, wherein the calcining conditions in the step (2) are as follows: the calcination temperature is 350-500 ℃, the calcination time is 2-4h, and the heating rate is 3-10 ℃/min.
4. The biochar-supported ionic liquid adsorbing material as claimed in claim 2, wherein the washing method in the step (2) comprises the following steps: adding the calcined peanut shell powder into absolute ethyl alcohol, and stirring for 2-4 h; wherein the ratio of the mass of the calcined peanut shell powder to the volume of the absolute ethyl alcohol is 1: 5-15.
5. The biochar-supported ionic liquid adsorbing material as claimed in claim 2, wherein the drying temperature of the step (1) is 55-65 ℃.
6. A preparation method of the biochar immobilized ionic liquid adsorbing material as defined in any one of claims 1 to 5, which is characterized by comprising the following steps:
(1) adding ionic liquid into an organic solvent, and stirring and mixing uniformly to obtain a mixed solution;
(2) adding the mixed solution into the peanut shell biochar, stirring and mixing uniformly, then carrying out ultrasonic treatment, filtering, washing and filtering again, and drying the obtained filter medium to obtain the biochar immobilized ionic liquid adsorbing material.
7. The method according to claim 6, wherein the organic solvent is one of methanol, ethanol, and acetone.
8. The method of claim 6, wherein the sonication time is between 0.5 and 1.5 hours.
9. The method of claim 6, wherein the drying conditions are: the drying temperature is 55-65 ℃, and the drying time is 8-24 h.
10. Use of the biochar-supported ionic liquid adsorbent material as claimed in any one of claims 1 to 5 in sewage treatment.
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