CN106957099B - Method for rapidly reducing and degrading triphenylmethane dye crystal violet wastewater - Google Patents
Method for rapidly reducing and degrading triphenylmethane dye crystal violet wastewater Download PDFInfo
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- CN106957099B CN106957099B CN201710228089.0A CN201710228089A CN106957099B CN 106957099 B CN106957099 B CN 106957099B CN 201710228089 A CN201710228089 A CN 201710228089A CN 106957099 B CN106957099 B CN 106957099B
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- C02F2101/00—Nature of the contaminant
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- C02F2101/308—Dyes; Colorants; Fluorescent agents
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- C—CHEMISTRY; METALLURGY
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Abstract
A method for rapidly reducing and degrading triphenylmethane dye crystal violet wastewater belongs to the field of nano materials and dye wastewater treatment. The preparation method comprises the steps of preparing nano zero-valent iron (perilla seed-nano zero-valent iron) by taking a perilla seed extracting solution as a stabilizer at room temperature, rapidly reducing and degrading triphenylmethane dye crystal violet under a suspension state, wherein the dose of the perilla seed-nano zero-valent iron suspension is 0.5-2.5g/L, the pH range of degraded dye wastewater is 2-10, the concentration range is 50-1000mg/L, the decolorization rate of 50-1000mg/L triphenylmethane dye crystal violet in 30min is at least 95.49% above, the removal rate of 500mg/L triphenylmethane dye crystal violet COD is 90.20%, and the preparation method has strong environmental adaptability, high degradation efficiency and complete degradation. The method is simple and rapid, and can achieve the aims of decoloring, degrading and removing organic pollutants of the dye in a short time.
Description
Technical Field
The invention belongs to the technical field of rapid reduction degradation treatment of dye wastewater, and particularly relates to application of a green synthesized nano zero-valent iron suspension by using a perilla seed extract to rapid reduction degradation of a dye in wastewater.
Background
In the conventional printing and dyeing industry, dye wastewater has strong visibility to affect the transparency of water and the transmittance of sunlight. The dye waste water is receiving attention because of its light, thermal stability and difficult biodegradability, and the degradation products are toxic and carcinogenic. Triphenylmethane dye Crystal Violet (CV) is a triphenylmethane dye, is a Crystal with metal luster or dark green crystalline powder in a green state when being solid, is a multi-benzene ring compound, and has a main structure that a central carbon atom is connected with three benzene rings. Crystal violet is widely used in cytology and bacteriology, is an excellent coloring agent, but because its color development is obvious, if discharge into the water can seriously influence the luminousness of water and threaten the growth of animals and plants in the water to cause environmental pollution and ecological destruction, simultaneously, crystal violet waste water COD is higher, and the biodegradability is poor, and the decoloration degree of difficulty is big, and effective degradation degree of difficulty is great, therefore triphenylmethane dye crystal violet waste water is urgent to need efficient degradation processing.
The traditional dye wastewater treatment methods including adsorption, ultrafiltration, chemical flocculation, ion exchange and other methods can effectively remove the dye in the wastewater, but the methods do not degrade dye molecules, only transfer the pollutants from a liquid phase to a solid phase to produce an enrichment effect on the pollutants, and if the treatment is improper, secondary pollution can be caused. The general advanced oxidation method has high requirements on equipment, high temperature resistance, high pressure resistance and corrosion resistance are often required, and the application cost is relatively high. Therefore, it is necessary to develop and research a dye degradation mode with simplicity, feasibility, mild reaction conditions and low operation cost so as to improve the degradation efficiency of the dye.
Since the discovery that iron filings can be used for in-situ remediation of water bodies, the technology of reducing pollutants in water bodies by zero-valent iron (ZVI) has been rapidly developed. ZVI has the advantages of low price, high speed, easy obtaining and the like, is widely applied to reduction and restoration of pollutants such as chlorohydrocarbon, chlorinated organic compounds, nitrogenous organic compounds, heavy metals and the like, and is also one of the commonly used media in Permeable Reactive Barriers (PRBs) technology. With the continuous development of nanotechnology, NZVI can degrade organic pollutants in water more rapidly, durably and thoroughly due to its larger specific surface area and reactivity than ZVI, and thus has gained more and more attention. For NZVI particles, it has been reported that the agglomeration and stability of NZVI are important factors affecting the use of NZVI, and bare NZVI loses activity because it is very easy to agglomerate, so in the process of preparing NZVI by a reduction reaction, it is often necessary to add a surface modifier, such as polyvinylpyrrolidone (PVP), carboxymethylcellulose (CMC), Tetrahydrofuran (THF), etc., to modify elementary iron particles, enhance the dispersibility thereof, prevent agglomeration, and thus synthesize surface-modified nano zero-valent iron, but the use of chemical reagents increases the synthesis cost and is harmful to the environment. The method for synthesizing the nano zero-valent iron by using the perilla seed extracting solution to replace chemical substances such as PVP, CMC, THF and the like as the surface modifier is feasible. The patent publication No. CN104174870A is a patent applied by Gaojing et al, wherein, it is mentioned that the method for synthesizing NZVI by using grape seed extract as surface modifier and applying it to the degradation of two active dyes of active brilliant red K-2G and active brilliant blue KN-R, the grape seed involved in the method is essentially different from the perilla seed used in the invention in terms of structure composition, the preparation steps are obviously simplified, and at the same time, the application effect of the synthesized perilla seed-nano zero-valent iron is not influenced, and the method has obvious progress, and in addition, the two dyes degraded in the patent publication No. CN104174870A belong to azo dyes and anthraquinone dyes respectively. Dyes are classified according to their properties and chemical structures, and may be classified into azo dyes, anthraquinone dyes, triphenylmethane dyes, indigoid dyes, sulfur dyes, and the like. Before the invention, reports of rapid reduction degradation of triphenylmethane crystal violet dye by utilizing nano zero-valent iron are not found.
The invention utilizes the green synthesized nano zero-valent iron of the perilla seeds to reduce and degrade the triphenylmethane dye, widens the material selection of the green synthesized nano zero-valent iron, simplifies the synthesis steps, develops a new method and a new thought for treating the triphenylmethane dye wastewater, provides a direction for rapidly and thoroughly degrading the triphenylmethane dye wastewater, provides a practical method for effectively preventing the triphenylmethane dye wastewater from being polluted, and has wide application significance.
The invention content is as follows:
the invention aims to provide a method for rapidly reducing and degrading triphenylmethane dye, and particularly relates to a method for reducing and degrading triphenylmethane dye by using a purple perilla seed green synthesized nano zero-valent iron suspension. The method firstly utilizes perilla seeds to synthesize nano zero-valent iron in a green way, and rapidly reduces and degrades triphenylmethane dye crystal violet by shaking under the conditions of normal temperature and normal pressure, is simple and rapid, and can achieve the purposes of dye decolorization, degradation and removal of dye organic pollutants in a short time.
The purpose of the invention is realized by the following technical scheme:
the invention provides a method for rapidly reducing and degrading triphenylmethane dye crystal violet wastewater, which is characterized by comprising the following steps of,
pulverizing sun-dried fructus Perillae, preparing fructus Perillae solution at 2g/L standard, performing ultrasound at 50W for 15min, filtering with filter paper (preferably medium-speed filter paper) to obtain fructus Perillae extractive solution, mixing with 0.1mol/L soluble divalent iron salt solution (2 wt%) containing Fe2+:BH4 -Slowly adding a borohydride solution under the condition that the molar ratio is 1:2, and stirring until no bubbles are generated, thereby obtaining the perilla seed surface modified nano zero-valent iron or a perilla seed-nano zero-valent iron suspension; under the condition of room temperature, the perilla seed-nano zero-valent ironAnd (3) adding the suspension into triphenylmethane dye crystal violet wastewater, and shaking to decolor and degrade the dye wastewater.
The perilla seed-nano zero-valent iron is suspension, and the dosage of the suspension directly applied to decoloration and degradation of dye wastewater is 0.5-2.5 g/L.
The method for rapidly reducing and degrading the triphenylmethane dye crystal violet wastewater is characterized by comprising the following steps of: the pH value of the dye wastewater is 2-10, and the concentration of the dye is 50-1000 mg/L.
The method for rapidly reducing and degrading the triphenylmethane dye crystal violet wastewater is characterized by comprising the following steps of: in the dye degradation process, the removal rate of COD of the dye wastewater of 500mg/L can reach 90.20%.
Compared with the prior art, the invention has the beneficial effects that:
1. the method for rapidly reducing and degrading the triphenylmethane dye crystal violet wastewater optimizes the process of green synthesis of the nano zero-valent iron by using the perilla seeds, so that the perilla seeds-nano zero-valent iron with good effect can be prepared more rapidly, simply and conveniently, the material selection range in the field of green synthesis is widened, the cost is low, and the method is environment-friendly.
2. The method for rapidly reducing and degrading the triphenylmethane dye crystal violet wastewater directly utilizes the perilla seed-nano zero-valent iron suspension to rapidly reduce and degrade the triphenylmethane dye crystal violet wastewater, does not need freeze-drying, reduces equipment requirements and greatly shortens time.
3. The method for rapidly reducing and degrading the triphenylmethane dye crystal violet wastewater has at least 95.49% of decolorization rate within 30min for 50-1000mg/L of triphenylmethane dye crystal violet, has good degradation effect under various pH conditions, has strong environmental adaptability, and proves the feasibility of applying the perilla seed-nano zero-valent iron to rapid reduction and degradation of the triphenylmethane dye.
4. The method for rapidly reducing and degrading the triphenylmethane dye crystal violet wastewater has a removal rate of 90.20% for COD of the triphenylmethane dye crystal violet of 500mg/L, and shows that the perilla seed-nano zero-valent iron can destroy and decompose a triphenylring structure in the triphenylmethane dye crystal violet, and the degradation degree is high.
Drawings
FIG. 1 is a graph showing the degradation curve of triphenylmethane dye crystal violet in the degradation wastewater of nano zero-valent iron synthesized in green by using perilla seeds in example 1;
FIG. 2 is a graph showing the degradation curve of triphenylmethane dye crystal violet in the degradation wastewater of nano zero-valent iron synthesized in green by using perilla seeds in example 2;
FIG. 3 is a graph showing the degradation curve of triphenylmethane dye crystal violet in the degradation wastewater of nano zero-valent iron synthesized in green by using perilla seeds in example 3;
FIG. 4 is a graph showing the degradation curve of triphenylmethane dye crystal violet in the degradation wastewater of nano zero-valent iron synthesized in green by using perilla seeds in example 4;
FIG. 5 is a graph showing the degradation curve of triphenylmethane dye crystal violet in the degradation wastewater of nano zero-valent iron synthesized in green by using perilla seeds in example 5;
FIG. 6 is a COD removal rate curve of triphenylmethane dye crystal violet in degradation wastewater of nano zero-valent iron synthesized by green purple perilla seeds in example 6.
Detailed Description
The present invention will be described in further detail with reference to specific examples, but the present invention is not limited to the examples.
Example 1
Sun-drying and air-drying fructus Perillae for 2 hr, pulverizing, preparing fructus Perillae solution at 2g/L standard, performing ultrasonic treatment at 50W for 15min, filtering with medium-speed filter paper to obtain fructus Perillae extractive solution, mixing with 100mL of 0.1mol/L soluble ferrous salt solution at 2 wt%, and mixing with Fe2+:BH4 -Slowly adding a borohydride solution under the condition that the molar ratio is 1:2, and stirring until no bubbles are generated, thereby obtaining the perilla seed surface modified nano zero-valent iron (perilla seed-nano zero-valent iron) suspension. Under the condition of room temperature, the perilla seed-nano zero-valent iron is added into 100mL of crystal violet wastewater containing 250mg/L of triphenylmethane dye with the pH value of 2 and the dosage of 1g/L, and the crystal violet wastewater is shaken to decolor the dye wastewaterAnd (4) degrading.
In the embodiment, the perilla seed-nano zero-valent iron completes the reduction and degradation of the triphenylmethane dye crystal violet in the wastewater within 25min, and the degradation efficiency is as high as 97.89%. FIG. 1 is a graph showing the degradation curve of the synthesized perilla seed-nano zero-valent iron to triphenylmethane dye crystal violet in wastewater.
Example 2
Sun-drying and air-drying fructus Perillae for 2 hr, pulverizing, preparing fructus Perillae solution at 2g/L standard, performing ultrasonic treatment at 50W for 15min, filtering with medium-speed filter paper to obtain fructus Perillae extractive solution, mixing with 100mL of 0.1mol/L soluble ferrous salt solution at 2 wt%, and mixing with Fe2+:BH4 -Slowly adding a borohydride solution under the condition that the molar ratio is 1:2, and stirring until no bubbles are generated, thereby obtaining the perilla seed surface modified nano zero-valent iron (perilla seed-nano zero-valent iron) suspension. Under the condition of room temperature, the perilla seed-nano zero-valent iron is added into 100mL of crystal violet wastewater containing 500mg/L triphenylmethane dye with pH of 4 in a dosage of 1.5g/L, and the crystal violet wastewater is shaken to decolor and degrade the dye wastewater.
In the embodiment, the perilla seed-nano zero-valent iron completes the reduction and degradation of the triphenylmethane dye crystal violet in the wastewater within 17.5min, and the degradation efficiency is up to 98.82%. Fig. 2 is a degradation curve of the purple triphenylmethane dye crystal in the wastewater by the perilla seed-nano zero-valent iron synthesized in the embodiment.
Example 3
Sun-drying and air-drying fructus Perillae for 2 hr, pulverizing, preparing fructus Perillae solution at 2g/L standard, performing ultrasonic treatment at 50W for 15min, filtering with medium-speed filter paper to obtain fructus Perillae extractive solution, mixing with 100mL of 0.1mol/L soluble ferrous salt solution at 2 wt%, and mixing with Fe2+:BH4 -Slowly adding a borohydride solution under the condition that the molar ratio is 1:2, and stirring until no bubbles are generated, thereby obtaining the perilla seed surface modified nano zero-valent iron (perilla seed-nano zero-valent iron) suspension. Adding the perilla seed-nano zero-valent iron into the mixture at the room temperature in a dosage of 0.5g/LAdding the mixture into crystal violet wastewater containing 50mg/L triphenylmethane dye with the pH value of 6 and 100mL, and shaking to decolor and degrade the dye wastewater.
In the embodiment, the perilla seed-nano zero-valent iron completes the reduction and degradation of the triphenylmethane dye crystal violet in the wastewater within 25min, and the degradation efficiency is up to 94.04%. FIG. 3 is a graph showing the degradation curve of the synthesized perilla seed-nano zero-valent iron to triphenylmethane dye crystal violet in wastewater.
Example 4
Sun-drying and air-drying fructus Perillae for 2 hr, pulverizing, preparing fructus Perillae solution at 2g/L standard, performing ultrasonic treatment at 50W for 15min, filtering with medium-speed filter paper to obtain fructus Perillae extractive solution, mixing with 100mL of 0.1mol/L soluble ferrous salt solution at 2 wt%, and mixing with Fe2+:BH4 -Slowly adding a borohydride solution under the condition that the molar ratio is 1:2, and stirring until no bubbles are generated, thereby obtaining the perilla seed surface modified nano zero-valent iron (perilla seed-nano zero-valent iron) suspension. Under the condition of room temperature, the perilla seed-nano zero-valent iron is added into 100mL of crystal violet wastewater containing 750mg/L of triphenylmethane dye with the pH value of 8 in a dosage of 2g/L, and the crystal violet wastewater is shaken to decolor and degrade the dye wastewater.
In the embodiment, the perilla seed-nano zero-valent iron completes the reduction and degradation of the triphenylmethane dye crystal violet in the wastewater within 27.5min, and the degradation efficiency is as high as 99.68%. FIG. 4 is a graph showing the degradation curve of the synthesized perilla seed-nano zero-valent iron to triphenylmethane dye crystal violet in wastewater.
Example 5
Sun-drying and air-drying fructus Perillae for 2 hr, pulverizing, preparing fructus Perillae solution at 2g/L standard, performing ultrasonic treatment at 50W for 15min, filtering with medium-speed filter paper to obtain fructus Perillae extractive solution, mixing with 100mL of 0.1mol/L soluble ferrous salt solution at 2 wt%, and mixing with Fe2+:BH4 -Slowly adding borohydride solution under the condition that the molar ratio is 1:2, stirring until no bubbles are generated, and obtaining the perilla seed surface modified nano zero-valent iron (perilla seed-nano zero-valent iron)Iron) suspension. Under the condition of room temperature, the perilla seed-nano zero-valent iron is added into 100mL of crystal violet wastewater containing 1000mg/L of triphenylmethane dye with the pH value of 10 in a dosage of 2.5g/L, and the crystal violet wastewater is shaken to decolor and degrade the dye wastewater.
In the embodiment, the perilla seed-nano zero-valent iron completes the reduction and degradation of the triphenylmethane dye crystal violet in the wastewater within 30min, and the degradation efficiency is as high as 99.45%. FIG. 5 is a graph showing the degradation curve of the synthesized perilla seed-nano zero-valent iron to triphenylmethane dye crystal violet in wastewater.
Example 6
Sun-drying and air-drying fructus Perillae for 2 hr, pulverizing, preparing fructus Perillae solution at 2g/L standard, performing ultrasonic treatment at 50W for 15min, filtering with medium-speed filter paper to obtain fructus Perillae extractive solution, mixing with 100mL of 0.1mol/L soluble ferrous salt solution at 2 wt%, and mixing with Fe2+:BH4 -Slowly adding a borohydride solution under the condition that the molar ratio is 1:2, and stirring until no bubbles are generated, thereby obtaining the perilla seed surface modified nano zero-valent iron (perilla seed-nano zero-valent iron) suspension. Under the condition of room temperature, the perilla seed-nano zero-valent iron is added into 100mL of crystal violet wastewater containing 500mg/L triphenylmethane dye with pH of 4 in a dosage of 1.0g/L, and the crystal violet wastewater is shaken to decolor and degrade the dye wastewater.
In the embodiment, the perilla seed-nano zero-valent iron completes the reduction and degradation of triphenylmethane dye crystal violet in the wastewater within 22.5min, and the degradation rate of dye COD is as high as 90.20%. A curve of COD removal rate of triphenylmethane dye crystal violet in wastewater by perilla seed-nano zero-valent iron.
Claims (5)
1. A method for rapidly reducing and degrading triphenylmethane dye crystal violet wastewater is characterized by comprising the following steps:
pulverizing sun-dried fructus Perillae, preparing fructus Perillae solution with 2g/L standard, performing ultrasonic treatment, filtering with filter paper to obtain fructus Perillae extractive solution, mixing with 0.1mol/L soluble ferrous salt solution, adding fructus Perillae extractive solutionThe mass percentage of the total mixed solution is 2 percent, and Fe is used2+:BH4 -Slowly adding a borohydride solution under the condition that the molar ratio is 1:2, and stirring until no bubbles are generated, thereby obtaining the perilla seed surface modified nano zero-valent iron or a perilla seed-nano zero-valent iron suspension; and (3) adding the perilla seed-nano zero-valent iron suspension into triphenylmethane dye crystal violet wastewater at room temperature, and oscillating to decolor and degrade the dye wastewater.
2. The method for rapidly reducing and degrading the triphenylmethane dye crystal violet wastewater according to claim 1, wherein the perilla seed-nano zero-valent iron is a suspension, and the dosage of the suspension directly applied to the decolorization and degradation of the dye wastewater is 0.5-2.5 g/L.
3. The method for rapidly reducing and degrading the triphenylmethane dye crystal violet wastewater according to claim 1, wherein the pH value of the dye wastewater is 2-10, and the dye concentration is 50-1000 mg/L.
4. The method for rapidly reducing and degrading the triphenylmethane dye crystal violet wastewater according to claim 1, wherein the ultrasonic conditions are as follows: and (4) carrying out ultrasonic treatment for 15min under the condition that the ultrasonic power is 50W.
5. The method for rapidly reducing and degrading the triphenylmethane dye crystal violet wastewater according to claim 1, wherein the COD removal rate of 500mg/L of dye wastewater in the dye degradation process reaches 90.20%.
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