CN112108126A - Passion fruit peel biological adsorbent for adsorbing anionic dye and preparation method and application thereof - Google Patents

Passion fruit peel biological adsorbent for adsorbing anionic dye and preparation method and application thereof Download PDF

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Publication number
CN112108126A
CN112108126A CN202011106036.XA CN202011106036A CN112108126A CN 112108126 A CN112108126 A CN 112108126A CN 202011106036 A CN202011106036 A CN 202011106036A CN 112108126 A CN112108126 A CN 112108126A
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passion fruit
fruit peel
reaction
raw material
preparation
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游少鸿
郑君里
陈凯伟
刘远立
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Guilin University of Technology
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Guilin University of Technology
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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
    • B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
    • B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
    • 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
    • C02F1/286—Treatment of water, waste water, or sewage by sorption using natural organic sorbents or derivatives thereof
    • 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
    • B01J2220/4825—Polysaccharides or cellulose materials, e.g. starch, chitin, sawdust, wood, straw, cotton
    • 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
    • C02F2101/308—Dyes; Colorants; Fluorescent agents

Abstract

The invention relates to the technical field of wastewater treatment, in particular to a passion fruit peel biological adsorbent for adsorbing anionic dye and a preparation method and application thereof. The preparation method comprises the following steps: performing alkali treatment on a passion fruit peel raw material to obtain a first passion fruit peel; mixing the first passion fruit peel with hydrogen peroxide, and carrying out oxidation reaction to obtain a second passion fruit peel; mixing the second passion fruit peel, an electrophilic reagent and epoxy chloropropane, and carrying out modification reaction to obtain a third passion fruit peel; mixing the third passion fruit peel with ethylenediamine, performing a first grafting reaction, adding triethylamine into the first grafting reaction system, and performing a second grafting reaction to obtain a fourth passion fruit peel; and mixing the fourth passion fruit peel with hydrochloric acid, carrying out protonation reaction, filtering, and drying a solid product to obtain the passion fruit peel biological adsorbent for adsorbing the anionic dye. The passion fruit peel biological adsorbent has good adsorption performance on anionic dye.

Description

Passion fruit peel biological adsorbent for adsorbing anionic dye and preparation method and application thereof
Technical Field
The invention relates to the technical field of wastewater treatment, in particular to a passion fruit peel biological adsorbent for adsorbing anionic dye and a preparation method and application thereof.
Background
With the continuous development of industry, the discharge of a large amount of colored wastewater seriously damages the environment, not only can influence the photosynthesis activity of aquatic organisms, but also can bring threat to the survival of animals and human beings. The textile, paper, plastic and cosmetic industries use a wide variety of anionic dyes to color products and discharge large amounts of waste water including dyes. Anionic dyes are toxic, have teratogenic, carcinogenic and mutagenic effects on humans and various organisms, and have serious environmental consequences. Therefore, how to better and more effectively treat the anionic dye wastewater becomes a difficulty in the field of water pollution control.
Disclosure of Invention
The invention aims to provide a passion fruit peel biological adsorbent for adsorbing anionic dye and a preparation method and application thereof.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a preparation method of passion fruit peel biological adsorbent for adsorbing anionic dye, which comprises the following steps:
performing alkali treatment on a passion fruit peel raw material to obtain a first passion fruit peel;
mixing the first passion fruit peel with hydrogen peroxide, and carrying out oxidation reaction to obtain a second passion fruit peel;
mixing the second passion fruit peel, an electrophilic reagent and epoxy chloropropane, and carrying out modification reaction to obtain a third passion fruit peel;
mixing the third passion fruit peel with ethylenediamine, performing a first grafting reaction, adding triethylamine into the first grafting reaction system, and performing a second grafting reaction to obtain a fourth passion fruit peel;
and mixing the fourth passion fruit peel with hydrochloric acid, carrying out protonation reaction, filtering, and drying a solid product to obtain the passion fruit peel biological adsorbent for adsorbing the anionic dye.
Preferably, the alkali liquor used for the alkali treatment is a sodium hydroxide solution or a potassium hydroxide solution; the concentration of the alkali liquor is 1-5 mol/L, and the dosage ratio of the passion fruit peel raw material to the alkali liquor is 1g (5-25) mL; the temperature of the alkali treatment is 80-100 ℃, and the time is 2-6 h.
Preferably, the dosage of the first passion fruit peel is calculated by the dosage of the passion fruit peel raw material, and the dosage ratio of the passion fruit peel raw material to hydrogen peroxide is 1g (5-15) mL; the temperature of the oxidation reaction is 80-100 ℃, and the time is 2-6 h.
Preferably, the dosage of the second passion fruit peel is calculated by the dosage of the passion fruit peel raw material, and the dosage ratio of the passion fruit peel raw material to the oxygen-containing chloropropane is 20g (1-5) mL; the temperature of the modification reaction is 80-100 ℃, and the time is 1-2 h.
Preferably, the dosage of the third passion fruit peel is calculated by the dosage of the passion fruit peel raw material, the dosage ratio of the passion fruit peel raw material to ethylenediamine is 20g (1-5) mL, and the dosage ratio of the passion fruit peel raw material to triethylamine is 4g (1-10) mL; the temperature of the first grafting reaction is 60-95 ℃, and the time is 1-2 h; the temperature of the second grafting reaction is 80-105 ℃, and the time is 1-5 h.
Preferably, the dosage of the fourth passion fruit peel is calculated by the dosage of the passion fruit peel raw material, the dosage ratio of the passion fruit peel to hydrochloric acid is 1g (5-25) mL, and the concentration of the hydrochloric acid is 1-5 mol/L.
Preferably, the temperature of the protonation reaction is room temperature, and the time is 1-5 h.
The invention provides the passion fruit peel biological adsorbent for adsorbing the anionic dye, which is prepared by the preparation method in the scheme.
The invention provides application of the passion fruit peel biological adsorbent for adsorbing the anionic dye in the scheme in adsorption of the anionic dye.
Preferably, the anionic dye comprises one or more of methyl orange, amaranth, lemon yellow, neo-carmine and chrome black.
The invention provides a preparation method of passion fruit peel biological adsorbent for adsorbing anionic dye, which comprises the following steps: performing alkali treatment on a passion fruit peel raw material to obtain a first passion fruit peel; mixing the first passion fruit peel with hydrogen peroxide, and carrying out oxidation reaction to obtain a second passion fruit peel; mixing the second passion fruit peel, an electrophilic reagent and epoxy chloropropane, and carrying out modification reaction to obtain a third passion fruit peel; mixing the third passion fruit peel with ethylenediamine, performing a first grafting reaction, adding triethylamine into the first grafting reaction system, and performing a second grafting reaction to obtain a fourth passion fruit peel; and mixing the fourth passion fruit peel with hydrochloric acid, carrying out protonation reaction, filtering, and drying a solid product to obtain the passion fruit peel biological adsorbent for adsorbing the anionic dye.
The method comprises the steps of performing alkali treatment on the passion fruit peel to remove pigments and pectin of the passion fruit peel and prevent the pigments and pectin from influencing adsorption of dyes, and then oxidizing the first passion fruit peel obtained after the alkali treatment by using hydrogen peroxide to remove the color of the passion fruit peel so as to prevent adverse influence on adsorption of anionic dyes; according to the method, ethylene diamine and triethylamine are sequentially adopted for grafting reaction, a large number of amino groups are grafted on the passion fruit peel, and the amino groups form active adsorption sites on the surface of a biological adsorbent, so that the physical adsorption and chemical adsorption reaction of an anionic dye on the surface of a biomass adsorbent are facilitated; and finally, protonating to improve the positive charge on the surface of the passion fruit peel and further improve the adsorption capacity of the passion fruit peel to anionic pollutants.
Compared with other modified adsorbents, the adsorbent prepared by the invention has the advantages of low cost, simple and convenient operation and easy water body separation, has good adsorption performance on methyl orange and amaranth at normal temperature, and can reach adsorption balance in a short time. In addition, the yellow passion fruit peel is agricultural and forestry waste, and the method can change waste into valuable.
Drawings
FIG. 1 is a scanning electron micrograph of the passion fruit peel biosorbent prepared in example 1;
FIG. 2 is a graph of the adsorption capacities of the passion fruit peel biosorbent prepared in example 1 for methyl orange and amaranth under different pH conditions;
FIG. 3 is the adsorption kinetics curves of the passion fruit peel biosorbent prepared in example 1 for methyl orange and amaranth;
FIG. 4 is the adsorption isotherms of the passion fruit peel biosorbent prepared in example 1 for methyl orange and amaranth;
FIG. 5 is a graph of the adsorption capacities of the passion fruit peel biosorbent prepared in example 1 for different dyes;
FIG. 6 is a graph showing the absorption spectra of the passion fruit peel biosorbent prepared in example 1 before and after adsorption of lemon yellow and methylene blue;
FIG. 7 is a graph showing the adsorption capacity of methyl orange by the passion fruit peel bioadsorbents prepared in examples 1-4 and comparative examples 1-2.
Detailed Description
The invention provides a preparation method of passion fruit peel biological adsorbent for adsorbing anionic dye, which comprises the following steps:
performing alkali treatment on a passion fruit peel raw material to obtain a first passion fruit peel;
mixing the first passion fruit peel with hydrogen peroxide, and carrying out oxidation reaction to obtain a second passion fruit peel;
mixing the second passion fruit peel, an electrophilic reagent and epoxy chloropropane, and carrying out modification reaction to obtain a third passion fruit peel;
mixing the third passion fruit peel with ethylenediamine, performing a first grafting reaction, adding triethylamine into the first grafting reaction system, and performing a second grafting reaction to obtain a fourth passion fruit peel;
and mixing the fourth passion fruit peel with hydrochloric acid, carrying out protonation reaction, filtering, and drying a solid product to obtain the passion fruit peel biological adsorbent for adsorbing the anionic dye.
In the present invention, the starting materials used are all commercially available products well known in the art, unless otherwise specified.
The invention carries out alkali treatment on the passion fruit peel raw material to obtain the first passion fruit peel.
In the invention, the passion fruit peel raw material is preferably yellow passion fruit peel. In the invention, the particle size of the passion fruit peel raw material is preferably 60-120 meshes, more preferably 80-110 meshes, and further preferably 90-100 meshes. In the invention, the alkali liquor used for the alkali treatment is preferably sodium hydroxide solution or potassium hydroxide solution, and more preferably sodium hydroxide solution; the concentration of the alkali liquor is preferably 1-5 mol/L, more preferably 2-3 mol/L, and most preferably 2 mol/L; the dosage ratio of the passion fruit peel raw material to the alkali liquor is preferably 1g (5-25) mL, more preferably 1g (10-20) mL, and most preferably 1g (20 mL). In the invention, the temperature of the alkali treatment is preferably 80-100 ℃, more preferably 90 ℃, and the time is preferably 2-6 h, more preferably 3-5 h, and most preferably 4 h.
In the invention, the alkali treatment process is preferably to mix and react the passion fruit peel raw material and alkali liquor. The invention removes the pigment and pectin of the passion fruit peel raw material by using alkali treatment, and the adsorption effect of the pigment and the pectin on the dye can be influenced.
After the alkali treatment, the method preferably further comprises the steps of carrying out suction filtration on the system subjected to the alkali treatment, and washing to be neutral to obtain the first passion fruit peel.
After the first passion fruit peel is obtained, the first passion fruit peel is mixed with hydrogen peroxide for oxidation reaction to obtain a second passion fruit peel.
In the invention, the dosage of the first passion fruit peel is calculated by the dosage of the passion fruit peel raw material, and the dosage ratio of the passion fruit peel raw material to hydrogen peroxide is preferably 1g (5-15) mL, more preferably 1g (7-12) mL, and most preferably 1g (10 mL). In the invention, the temperature of the oxidation reaction is preferably 80-100 ℃, and more preferably 90 ℃; the time is preferably 2 to 6 hours, more preferably 3 to 5 hours, and most preferably 4 hours.
In the invention, the mixing mode of the first passion fruit peel and hydrogen peroxide is preferably as follows: and dropwise adding the hydrogen peroxide into the first passion fruit peel. The invention adopts a dropwise adding mode to prevent potential safety hazard caused by one-time adding violent reaction.
After the oxidation reaction is finished, the method preferably further comprises the steps of carrying out suction filtration on a system after the oxidation reaction, washing to be neutral, and drying to obtain the second passion fruit peel. The drying conditions of the present invention are not particularly limited, and those well known in the art may be used. The method utilizes hydrogen peroxide to oxidize the first passion fruit peel, can remove the color of the peel and prevent the adverse effect on the adsorption of anionic dyes.
After the second passion fruit peel is obtained, the second passion fruit peel, an electrophilic reagent and epoxy chloropropane are mixed for modification reaction to obtain a third passion fruit peel.
In the present invention, the electrophile is preferably Dimethylformamide (DMF), ethanol or dimethyl sulfoxide (DMSO), more preferably DMF.
In the invention, the dosage of the second passion fruit peel is calculated by the dosage of the passion fruit peel raw material, and the dosage ratio of the passion fruit peel raw material to the oxygen-containing chloropropane is preferably 20g (1-5) mL, more preferably 20g (2-4) mL, and most preferably 20g:3 mL; the dosage ratio of the passion fruit peel to the electrophilic reagent is preferably 2g (1-5) mL, and more preferably 1g:2.5 mL.
The preparation method preferably comprises the steps of mixing the second passion fruit peel with an electrophilic reagent, placing the mixture in a water bath kettle at the temperature of 80-100 ℃, and then adding epoxy chloropropane for modification reaction. In the invention, the temperature of the modification reaction is preferably 80-100 ℃, more preferably 90 ℃, and the time is preferably 1-2 h, more preferably 2 h.
In the modification reaction process, under the action of an electrophilic reagent, epichlorohydrin firstly opens a ring and then reacts with a hydroxyl group of C6 on the passion fruit. The invention uses epoxy chloropropane as tie for grafting ethylenediamine and triethylamine.
After the third passion fruit peel is obtained, the third passion fruit peel and ethylenediamine are mixed to perform a first grafting reaction, and then triethylamine is added into the first grafting reaction system to perform a second grafting reaction to obtain a fourth passion fruit peel.
In the invention, the dosage of the third passion fruit peel is calculated by the dosage of the passion fruit peel raw material, and the dosage ratio of the passion fruit peel raw material to ethylenediamine is preferably 20g (1-5) mL, more preferably 20g (1-3) mL, and most preferably 20g:1 mL; the dosage ratio of the passion fruit peel raw material to triethylamine is preferably 4g (1-10) mL, more preferably 4g (1-5) mL, and most preferably 4g:2 mL.
In the invention, the time of the first grafting reaction is preferably 1-2 h, and more preferably 1 h; the temperature of the first grafting reaction is preferably 60-95 ℃, more preferably 70-90 ℃, and most preferably 85-90 ℃.
In the invention, the time of the second grafting reaction is preferably 1-5 h, and more preferably 2-3 h; the temperature of the second grafting reaction is preferably 80-105 ℃, more preferably 85-100 ℃, and most preferably 90-95 ℃.
In the first grafting reaction process, epichlorohydrin continues to perform ring-opening reaction, the amine group of ethylenediamine reacts with the other end group of the epichlorohydrin ring to graft the third passion fruit peel, and then in the second grafting reaction process, under the condition that the epichlorohydrin is slightly excessive, triethylamine reacts with the other amino group of the ethylenediamine under the crosslinking of the epichlorohydrin to obtain the fourth passion fruit peel. N of triethylamine+NH relative to ethylenediamine2The groups are more active, and the adsorption of the anionic dye is more facilitated.
The surface of the fourth passion fruit peel obtained after the grafting reaction contains a large amount of amino groups, and the fourth passion fruit peel can be used as an active site for adsorbing an anionic dye, and is beneficial to the performance of a physical adsorption reaction and a chemical adsorption reaction.
After the fourth passion fruit peel is obtained, the fourth passion fruit peel is mixed with hydrochloric acid for protonation reaction, and after solid products are filtered and dried, the passion fruit peel biological adsorbent for adsorbing anionic dye is obtained.
In the invention, the dosage of the fourth passion fruit peel is calculated by the dosage of the passion fruit peel raw material, and the dosage ratio of the passion fruit peel to the hydrochloric acid is preferably 1g (5-25) mL, more preferably 1g (10-20) mL, and most preferably 1g:10 mL; the concentration of the hydrochloric acid is preferably 1-5 mol/L, and more preferably 1 mol/L.
The invention has no special requirements on the mixing process of the fourth passion fruit peel and the hydrochloric acid, and the mixing process which is well known in the field can be adopted. In the present invention, the protonation reaction is preferably carried out at room temperature; the time of the protonation reaction is preferably 1-5 h, and more preferably 1 h.
The invention utilizes the protonation reaction to improve the amount of positive charges on the surface of the passion fruit peel, thereby further improving the adsorption effect on the anionic dye.
The invention adopts hydrochloric acid to carry out protonation reaction, can improve the activity of amino on the surface of the adsorbent, accelerate the adsorption rate and improve the adsorption effect, and has better adsorption effect compared with other acids.
The present invention has no special requirement on the filtering process, and the filtering process known in the field can be adopted. The present invention preferably further comprises washing the filtered solid product with distilled water after filtration. The washing process of the present invention is not particularly limited, and washing processes well known in the art may be used. The present invention has no special requirement for the drying process, and the drying process known in the field can be adopted.
The invention provides the passion fruit peel biological adsorbent for adsorbing the anionic dye, which is prepared by the preparation method in the scheme. The passion fruit peel bio-adsorbent contains a large amount of amino groups, and the amino groups form active adsorption sites on the surface of the bio-adsorbent, so that the physical adsorption and chemical adsorption reaction of anionic dye on the surface of the biomass adsorbent can be favorably carried out; the passion fruit peel bio-adsorbent also contains a large amount of positive charges, so that the adsorption capacity of the passion fruit peel to anionic pollutants can be further improved.
The invention provides application of the passion fruit peel biological adsorbent for adsorbing the anionic dye in the scheme in adsorption of the anionic dye. In the present invention, the anionic dye preferably includes one or more of methyl orange, amaranth, lemon yellow, neo-carmine, and chrome black. In the present invention, the method of application preferably comprises the steps of: adding the passion fruit peel biological adsorbent into a solution containing an anionic dye, and carrying out adsorption reaction under the stirring condition.
In the invention, the concentration of the anionic dye in the solution containing the anionic dye is preferably 50-2000 mg/L, and in the embodiment of the invention, the concentration is specifically 50mg/L, 100mg/L, 150mg/L, 200mg/L, 250mg/L, 300mg/L, 400mg/L, 500mg/L, 600mg/L, 700mg/L, 800mg/L, 900mg/L, 1000mg/L or 2000 mg/L. In the present invention, the pH of the solution containing the anionic dye is preferably 4 to 11, and more preferably 4 to 6. In the invention, the dosage of the passion fruit peel biological adsorbent is preferably 0.1-5 g/L, and more preferably 0.5-2 g/L.
In the present invention, the rotation speed of the stirring is preferably 100 to 200rpm, and more preferably 180 rpm. In the invention, the temperature of the adsorption reaction is preferably 20-30 ℃, and more preferably 25 ℃. In the present invention, the time of the adsorption reaction is preferably 15min or more, more preferably 15min to 5 hours, further preferably 0.5 to 5 hours, and most preferably 2 to 4 hours.
The passion fruit peel biosorbent for adsorbing anionic dye and the preparation method and application thereof provided by the invention are described in detail with reference to the following examples, but the examples should not be construed as limiting the scope of the invention.
Example 1
Placing 20g of yellow passion fruit peel powder which is sieved by a 100-mesh sieve in a beaker, adding the yellow passion fruit peel powder into a 2M NaOH solution for alkali treatment, wherein the volume of the NaOH solution is 400mL, the reaction temperature is 90 ℃, the reaction is carried out for 4 hours, suction filtration and washing are carried out until the solution is neutral, placing the obtained first passion fruit peel in a three-neck bottle, dropwise adding 200mL of hydrogen peroxide at the temperature of 90 ℃, reacting for 4 hours, suction filtration and washing until the solution is neutral, and drying to obtain second passion fruit peel;
putting the second passion fruit peel into a two-mouth bottle, adding 25mL of DMF, putting into a water bath kettle at 90 ℃, adding 3mL of epichlorohydrin, and carrying out modification reaction for 2h to obtain a third passion fruit peel;
adding 1mL of ethylenediamine into the third passion fruit peel, performing a first grafting reaction for 1h at 90 ℃, then adding 10mL of triethylamine, performing a second grafting reaction for 2h at 90 ℃, performing suction filtration, washing and drying to obtain a fourth passion fruit peel;
and mixing the fourth passion fruit peel with 200mL of 1M hydrochloric acid at room temperature, carrying out protonation reaction for 1 hour, filtering, washing with distilled water, and drying to obtain the passion fruit peel biological adsorbent for adsorbing the anionic dye.
Fig. 1 is a scanning electron micrograph of the passion fruit peel biosorbent prepared in example 1, and it can be seen from fig. 1 that the passion fruit peel biosorbent prepared by the invention has a smooth and non-porous surface and an irregular structure, which indicates that the adsorption process is not a porous physical adsorption.
Examples 2 to 4
The difference from example 1 is only that triethylamine was used in an amount of 5mL, 7.5mL and 12.55mL in this order.
Comparative example 1
The only difference from example 1 is that triethylamine was used in an amount of 0.
Comparative example 2
The only difference from example 1 is that triethylamine was used in an amount of 2.5 mL.
Comparative example 3
The only difference from example 1 is that hydrochloric acid is changed to sulfuric acid.
Comparative example 4
The only difference from example 1 is that no protonation reaction was carried out.
Application example 1
10mL of initial solution of methyl orange and amaranth with the concentration of 2000mg/L are respectively transferred and placed in a 50mL centrifuge tube, the pH value of the solution is adjusted by 0.1mol/L NaOH solution or 0.1mol/L HCl solution, 5mg of the passion fruit peel biological adsorbent prepared in the embodiment 1 is added, the mixture is subjected to constant-temperature shaking adsorption for 240min at the room temperature and at the speed of 180rmp, the mixture is centrifuged in a 11000r/min centrifuge, supernatant liquid is taken, and the concentration of the methyl orange and the amaranth in the supernatant liquid is measured by a spectrophotometry method, and the result is shown in the attached figure 2 (in the figure 2, MO represents the methyl orange, ART represents the amaranth), and the specific result is shown in the table 1.
TABLE 1 adsorption capacities (mg/g) for methyl orange and amaranth at different pH values
pH=4 pH=5 pH=6 pH=7 pH=8 pH=9 pH=10 pH=11
Methyl orange 1687 1455 1224 1192 1187 1157 1019 438
Amaranth 970 947 923 872 852 822 681 79
As can be seen from fig. 2 and table 1, the passion fruit peel bio-adsorbent prepared by the invention has a larger adsorption capacity under an acidic condition than under an alkaline condition, and particularly has a better adsorption performance under a condition of a pH value of 4-6.
Application example 2
Respectively transferring 300mL of methyl orange and amaranth with the concentration of 200mg/L into a 500mL beaker, adding 50mg of passion fruit peel bio-adsorbent prepared in example 1, adding a stirrer, adjusting the pH value of the solution to 5 by using 0.1mol/L NaOH solution or 0.1mol/L HCl solution, directly placing the solution into a constant-temperature water bath kettle, adjusting the temperature to 25 ℃, stirring at 180rmp, sampling at intervals of 0.5, 1, 2, 3, 5, 10, 15, 20, 25, 30, 40, 50, 60, 70, 80, 90, 100, 110, 120, 130, 140, 150, 160, 170 and 180min, placing 3mL of the solution into a centrifuge tube at the same position, centrifuging at 11000r/min, taking supernatant, and measuring the concentrations of the methyl orange and the amaranth in the supernatant by using a spectrophotometric method, wherein the result is shown in the attached drawing 3.
As can be seen from FIG. 3, the adsorption gradually reaches equilibrium along with the extension of the adsorption time, and reaches equilibrium when the adsorption time is 2 hours, which shows that the passion fruit peel bio-adsorbent prepared by the invention can reach equilibrium in a short time.
Application example 3
Transferring 20mL of methyl orange and amaranth with different concentrations into a 100mL polyethylene plastic bottle, wherein the concentrations are respectively 50, 100, 150, 200, 250, 300, 400, 500, 600, 700, 800, 900 and 1000mg/L, adding 10mg of passion fruit peel bio-adsorbent prepared in example 1, adjusting the pH value of the solution to be 5 by 0.1mol/L NaOH solution or 0.1mol/L HCl solution, placing the solution in a constant temperature shaking table, adjusting the temperature to be 25 ℃, rotating speed to be 180rmp and shaking time to be 4h, then taking 10mL of sample into a centrifuge tube, centrifuging the sample in a 11000r/min centrifuge, taking supernatant, and measuring the concentrations of methyl violet and methylene blue in the supernatant by adopting a spectrophotometry method, wherein the result is shown in figure 4.
As can be seen from FIG. 4, the maximum adsorption capacity of the passion fruit peel bio-adsorbent prepared in example 1 for methyl orange is 1455mg/g, and the maximum adsorption capacity for amaranth is 970 mg/g.
Application example 4
Transferring 10mL of Methyl Orange (MO), Amaranth (ART), New Carmine (NC), lemon yellow (TTZ), chrome black R (MB 17), Methyl Violet (MV) and Methylene Blue (MB) into a 100mL polyethylene plastic bottle, wherein the concentration is 1000mg/L, adding 5mg of the passion fruit peel bio-adsorbent prepared in example 1, adjusting the pH value of the solution to be 5 by 0.1mol/L NaOH solution or 0.1mol/L HCl solution, placing the solution in a constant temperature shaking table, adjusting the temperature to be 25 ℃, rotating the speed to be 180rmp, shaking the time to be 4h, then placing 10mL of a sample into a centrifuge tube, centrifuging the sample in a 11000R/min centrifuge, taking supernatant, and measuring the concentration in the supernatant by a spectrophotometry method, wherein the result is shown in figure 5.
As can be seen from FIG. 5, the passion fruit peel biosorbent of the present invention has an adsorption capacity of 1455.274mg/g for MO, 947.51463mg/g for ART, 945.29902mg/g for NC, 822.11039mg/g for TTZ, 717.55604mg/g for MB17, 36.02146mg/g for MV and 33.92171mg/g for MB), which indicates that the passion fruit peel biosorbent prepared by the present invention has a good adsorption effect on anionic dyes and a poor adsorption effect on cationic dyes.
Application example 5
Transferring 5mL of lemon yellow and methylene blue into a 10mL centrifuge tube respectively, measuring the absorption peak of the mixed solution, adding 50mg of passion fruit peel bio-adsorbent prepared in example 1, adjusting the pH value of the solution to 5 by 0.1mol/L of NaOH solution or 0.1mol/L of HCl solution, placing the solution in a constant temperature shaking table, adjusting the temperature to 25 ℃, rotating speed to 180rmp, shaking for 4h, then taking 10mL of sample into the centrifuge tube, centrifuging in a 11000r/min centrifuge, taking the supernatant, and measuring the absorption peak of the supernatant, wherein the result is shown in figure 6.
As can be seen from fig. 6, after the passion fruit peel bio-adsorbent prepared by the method disclosed by the invention is added, the absorption peak of the anionic dye lemon yellow disappears, and the absorption peak of the cationic dye methylene blue does not change significantly, which indicates that the passion fruit peel bio-adsorbent disclosed by the invention can selectively absorb the anionic dye.
Application example 6
The passion fruit bioadsorbents prepared in examples 1-4 and comparative examples 1-2 were tested for adsorption performance, and the specific steps were as follows: transferring 10mL of methyl orange solution with initial concentration of 1000mg/L into a 50mL centrifuge tube, adjusting the pH value of the solution to 5 by 0.1mol/L NaOH solution or 0.1mol/L HCl solution, adding 5mg of passion fruit peel bio-adsorbent, oscillating and adsorbing at constant temperature at 180rmp rotation speed for 240min at room temperature, centrifuging in a 11000r/min centrifuge, taking supernatant, and measuring the concentration of methyl orange in the supernatant by adopting a spectrophotometry method, wherein the result is shown in figure 7. In FIG. 7, A0 represents the amount of triethylamine used as 0, A2.5 represents the amount of triethylamine used as 2.5mL, and so on. As can be seen from fig. 7, when triethylamine was not added or the amount of triethylamine used was small, the adsorption effect on the anionic dye was poor.
Application example 7
The passion fruit biosorbents prepared in the example 1 and the comparative examples 3-4 are subjected to adsorption performance tests, and the specific steps are as follows: transferring 10mL of methyl orange solution with the initial concentration of 1000mg/L into a 50mL centrifuge tube, adjusting the pH value of the solution to be 5 by 0.1mol/L NaOH solution or 0.1mol/L HCl solution, adding 5mg of passion fruit peel bio-adsorbent, oscillating and adsorbing at constant temperature at 180rmp rotation speed for 240min at room temperature, centrifuging in a 11000r/min centrifuge, taking supernatant, measuring the absorbance of the methyl orange in the supernatant by adopting a spectrophotometry method, and calculating the adsorption quantity. The results show that the maximum adsorption amount of methyl orange by the passion fruit peel biosorbent obtained by the non-protonation reaction in the comparative example 4 is 748mg/g, the maximum adsorption amount of methyl orange by the passion fruit peel biosorbent obtained by the protonation reaction in the example 1 is 1455mg/g, and the maximum adsorption amount of methyl orange by the passion fruit peel biosorbent obtained by the protonation reaction in the comparative example 3 is 987 mg/g.
The embodiments show that the passion fruit peel biological adsorbent prepared by the invention has good adsorbability and selectivity on anionic dyes, and can reach adsorption balance in a short time.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.

Claims (10)

1. A preparation method of passion fruit peel biological adsorbent for adsorbing anionic dye is characterized by comprising the following steps:
performing alkali treatment on a passion fruit peel raw material to obtain a first passion fruit peel;
mixing the first passion fruit peel with hydrogen peroxide, and carrying out oxidation reaction to obtain a second passion fruit peel;
mixing the second passion fruit peel, an electrophilic reagent and epoxy chloropropane, and carrying out modification reaction to obtain a third passion fruit peel;
mixing the third passion fruit peel with ethylenediamine, performing a first grafting reaction, adding triethylamine into the first grafting reaction system, and performing a second grafting reaction to obtain a fourth passion fruit peel;
and mixing the fourth passion fruit peel with hydrochloric acid, carrying out protonation reaction, filtering, and drying a solid product to obtain the passion fruit peel biological adsorbent for adsorbing the anionic dye.
2. The preparation method according to claim 1, wherein the alkali solution used for the alkali treatment is a sodium hydroxide solution or a potassium hydroxide solution; the concentration of the alkali liquor is 1-5 mol/L, and the dosage ratio of the passion fruit peel raw material to the alkali liquor is 1g (5-25) mL; the temperature of the alkali treatment is 80-100 ℃, and the time is 2-6 h.
3. The preparation method of claim 1, wherein the dosage of the first passion fruit peel is calculated by the dosage of a passion fruit peel raw material, and the dosage ratio of the passion fruit peel raw material to hydrogen peroxide is 1g (5-15) mL; the temperature of the oxidation reaction is 80-100 ℃, and the time is 2-6 h.
4. The preparation method according to claim 1, wherein the amount of the second passion fruit peel is calculated by the amount of the passion fruit peel raw material, and the ratio of the passion fruit peel raw material to the oxygen-containing chloropropane is 20g (1-5) mL; the temperature of the modification reaction is 80-100 ℃, and the time is 1-2 h.
5. The preparation method according to claim 1, wherein the amount of the third passion fruit peel is calculated by the amount of the passion fruit peel raw material, the amount ratio of the passion fruit peel raw material to ethylenediamine is 20g (1-5) mL, and the amount ratio of the passion fruit peel raw material to triethylamine is 4g (1-10) mL; the temperature of the first grafting reaction is 60-95 ℃, and the time is 1-2 h; the temperature of the second grafting reaction is 80-105 ℃, and the time is 1-5 h.
6. The preparation method of claim 1, wherein the consumption of the fourth passion fruit peel is calculated by the consumption of the passion fruit peel raw material, the consumption ratio of the passion fruit peel to the hydrochloric acid is 1g (5-25) mL, and the concentration of the hydrochloric acid is 1-5 mol/L.
7. The preparation method according to claim 6, wherein the protonation reaction is carried out at room temperature for 1-5 h.
8. The passion fruit peel bio-adsorbent for adsorbing anionic dye prepared by the preparation method of any one of claims 1 to 7.
9. The use of the passion fruit peel biosorbent adsorbing anionic dyes of claim 8 to adsorb anionic dyes.
10. Use according to claim 9, wherein the anionic dye comprises one or more of methyl orange, amaranth, lemon yellow, neo-carmine and chrome black.
CN202011106036.XA 2020-10-15 2020-10-15 Passion fruit peel biological adsorbent for adsorbing anionic dye and preparation method and application thereof Pending CN112108126A (en)

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