CN112551634A - Method for treating FOX-7 synthetic wastewater by using zero-dimensional carbon-based nano material - Google Patents
Method for treating FOX-7 synthetic wastewater by using zero-dimensional carbon-based nano material Download PDFInfo
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Abstract
The invention discloses a treatment method of FOX synthetic wastewater. The method adopts zero-dimensional carbon-based nano materials to carry out photocatalytic treatment on the FOX synthetic wastewater under the conditions of illumination and electrification. The main component contained in the FOX-7 synthetic wastewater is dimethyl sulfoxide which is a universal solvent, and the wastewater treatment or utilization technologies thereof have defects of different degrees. The zero-dimensional carbon-based nano material is used for treating FOX-7 synthetic simulation wastewater, provides a green synthetic production process for synthesizing FOX-7 energetic materials, and effectively promotes the industrial production process of FOX-7 energetic material products.
Description
Technical Field
The invention belongs to the technical field of water treatment, and particularly relates to a method for treating FOX-7 synthetic wastewater by using a zero-dimensional carbon-based nano material.
Background
FOX-7(1, 1-diamino-2,2-dinitroethylene, DADE for short) is a high-energy insensitive explosive, which is one of the research hotspots for explosive synthesis after being publicly reported in 1998. At present, the domestic synthetic research of FOX-7 is limited to laboratory research and pilot test production scale, and no industrial production is seen. In the research process of synthesis and production, the process contents of the production process of FOX-7, product quality, yield and the like are mainly researched, the control of the production and synthesis process is concerned, the pollution condition of pollutants generated in each process technology link in the synthesis and production process to the environment is not researched or reported, and more importantly, the treatment of the FOX-7 synthesis wastewater is not concerned. How to effectively treat synthetic wastewater in the production of FOX-7 and provide technical support guarantee for the subsequent green synthesis of FOX-7 becomes a technical problem to be solved urgently.
Disclosure of Invention
The invention provides a treatment method of FOX synthetic wastewater, which comprises the following steps: the FOX synthetic wastewater is subjected to photocatalytic treatment by adopting a zero-dimensional carbon-based nano material under the conditions of illumination and electrification.
According to the technical scheme of the invention, the FOX synthetic wastewater contains dimethyl sulfoxide, and the volume percentage of the dimethyl sulfoxide is 0.2-0.8%, such as 0.3-0.7%, 0.4-0.6%, and exemplarily 0.45%. Further, the FOX synthetic wastewater can also contain nitric acid; the concentration of the nitric acid in the wastewater is very low, for example, the nitric acid is the residue of the reactants in the synthesis step and the concentration can reach 0.01 wt% at most. Furthermore, the FOX synthetic wastewater can also contain sulfuric acid; the concentration of the sulfuric acid in the waste water is very low, for example, the sulfuric acid is the reactant residue in the synthesis step, and the concentration can reach 0.01 wt% at most.
According to the technical scheme of the invention, the zero-dimensional carbon-based nano material is selected from a nano diamond material, and is preferably a nano diamond film. Further, the nanodiamond material, nanodiamond film, may be prepared by methods known in the art; for example, a nano-diamond film is prepared from nano-diamond as a sheet-like film material; specifically, the compound can be prepared by the method in CN 201910343098.3.
According to the technical scheme of the invention, the illumination condition comprises the following steps: and (5) natural illumination.
According to an aspect of the present invention, the energization condition includes: the current is 10-15A, the alternating voltage is 200-250V, and the continuous electrification is realized; for example, the current 12A, 220V AC voltage, and continuous current.
According to the technical scheme of the invention, the processing process comprises the following steps: the zero-dimensional carbon-based nano material is prepared into a film or coated on a carrier in a film form, and is immersed in FOX synthetic wastewater to enable a water body to be in a flowing state, and a photocatalytic reaction is carried out under the conditions of natural illumination and electrification. The carrier can be selected by those skilled in the art according to actual needs, for example, a plate-like object or a cylinder-like object, which is beneficial for the zero-dimensional carbon-based nanomaterial to fully contact with the water body.
In the prior art, the treatment method for the wastewater containing mixed acid of nitric acid and sulfur mainly adopts acid-base neutralization, and quantitative alkali is added into the wastewater to carry out acid-base neutralization, and then the wastewater can be collected and discharged. The solvent contained in the waste water can be separated or purified and recycled by adopting a liquid-liquid separation technology, and the liquid-liquid separation technology mainly comprises distillation, reduced pressure distillation, membrane technology and extraction. However, the hydrolysis solvent in the FOX synthetic wastewater is mainly DMF/H2O、DMSO/H2O and NMP/H2And O is an organic solvent with good solubility, and the separation method adopting extraction, membrane technology and membrane distillation cannot achieve good separation and treatment effects because the solubility of the O has certain influence on the organic solvent and membrane materials.
The invention adopts the synergistic ultra-purification technology based on the zero-dimensional carbon-based nano material to treat the synthetic wastewater containing FOX for the first time. Based on the special structure, the electrode framework and the high-efficiency photocatalytic performance of the zero-dimensional carbon-based nano material, the material generates high-efficiency self-absorption and interaction under illumination to form the carbon quantum dots. The carbon quantum dots are a novel globular zero-dimensional carbon-based material, have the size of below 10nm, mainly consist of C, H, O, N four elements, and the content of C, O is high. The carbon quantum dots are also a novel high-efficiency photocatalyst, and have excellent optical properties and good water solubility. When one or more of N, S, Si, Se, P, As, B and other atoms are doped in the carbon quantum dots, the carbon dots can generate high-efficiency photocatalytic oxidation reaction within the visible light spectrum range (300-850 nm). Under the irradiation of sunlight, the carbon quantum dots efficiently decompose water, generate hydrogen, oxygen, hydroxyl free radicals and the like, and efficiently digest organic pollutants in the environment.
The zero-dimensional carbon-based nano material is contacted with the FOX-7 synthetic wastewater to form cooperative integration with water. The zero-dimensional carbon-based nano material overflows high-concentration negative affinity electrons under the drive of an alternating-current low-voltage electric field, and the overflowed electrons form a synergistic resonance state with a certain frequency in the environment of water molecule vibration frequency. The activated water molecules are reduced to a state with higher energy, and the original activity of the water molecules is recovered to become small molecular water clusters. The released electrons have low kinetic energy and high potential energy, can not only decompose water molecules to generate active oxygen, oxygen and the like, but also can effectively act on an interaction interface state between molecular groups absorbed together in a complex state in water to disperse a complex (dimethyl sulfoxide) in the water body to form a large number of molecular structure carbon quantum dots taking carbon as a main framework. Through the electrode framework of the carbon quantum dots and the high-efficiency photocatalytic performance of the carbon quantum dots, solar energy is absorbed to generate photocatalytic reaction under the illumination condition, and water molecules are decomposed to generate active oxygen and hydrogen. Hydrogen becomes the energy currency of the microorganisms. The active oxygen is further reacted into hydroxyl free radical and other oxidizing radicals to degrade pollutant fast. Meanwhile, negative affinity low-energy electrons emitted by the zero-dimensional carbon-based nano material continue to carry out photodegradation and photocatalysis on the water body in the treatment process, so that the water body purification capacity is quickly recovered.
The invention has the beneficial effects that:
the zero-dimensional carbon-based nano material has a good effect on the treatment of the FOX-7 synthetic wastewater, and provides a novel treatment technology for the treatment of the FOX-7 synthetic wastewater. The main component contained in the FOX-7 synthetic wastewater is dimethyl sulfoxide which is a universal solvent, and the wastewater treatment or utilization technologies thereof have defects of different degrees. The zero-dimensional carbon-based nano material is used for treating FOX-7 synthetic simulation wastewater, provides a green synthetic production process for synthesizing FOX-7 energetic materials, and effectively promotes the industrial production process of FOX-7 energetic material products.
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FIG. 1 is a graph showing the change of COD index in FOX-7 synthesis simulation wastewater treatment in example 1.
Detailed Description
The technical solution of the present invention will be further described in detail with reference to specific embodiments. It is to be understood that the following examples are only illustrative and explanatory of the present invention and should not be construed as limiting the scope of the present invention. All the technologies realized based on the above-mentioned contents of the present invention are covered in the protection scope of the present invention.
Unless otherwise indicated, the raw materials and reagents used in the following examples are all commercially available products or can be prepared by known methods.
Experimental materials:
dimethyl sulfoxide (chemically pure), nitric acid (chemically pure), sulfuric acid (chemically pure).
The preparation process of the nano-diamond film (refer to the CN201910343098.3 process) comprises the following steps:
s1: carrying out surface nitriding treatment on the metal workpiece substrate;
s2: cleaning the surface of a metal workpiece substrate by using gas-phase plasma under a low-pressure condition;
s3: introducing carbon, nitrogen and sulfur source gas and hydrogen diluted by inert gas under the condition of low pressure, and depositing a diamond film layer on the metal workpiece substrate by utilizing a radio frequency plasma chemical vapor deposition mode;
adding a nitrogen element-containing and sulfur element-containing doping gas component in the process of depositing the diamond film, wherein the proportion of the nitrogen element-containing doping gas component is 1.0%; the nitrogen element doping gas is ethylenediamine;
the gas pressure is 8Torr and the heating temperature is 200 ℃ in the process of depositing the diamond film;
applying high-frequency electromagnetic wave with frequency of 1000MHz and power of 50W/cm to the plasma in the process of depositing the diamond coating2；
S4: heating the metal workpiece substrate for 30-60 minutes, continuously utilizing inert gas diluted carbon, nitrogen and sulfur source gas and hydrogen radio frequency plasma chemical vapor deposition diamond coating layers on the diamond coating layers deposited on the metal workpiece substrate, and heating the newly deposited coating layers for 30-60 minutes;
s5: and repeating the step S4 for multiple times to deposit a plurality of diamond films on the surface of the metal workpiece substrate.
Example 1
2500mL of dimethyl sulfoxide was dissolved in 550L of tap water, and nitric acid (0.01 wt%) and sulfuric acid (0.01 wt%) were added thereto and mixed uniformly to prepare FOX-7 synthetic wastewater. Immersing a workpiece containing the nano-diamond film in FOX-7 synthetic simulation wastewater, stirring to enable a water body to be in a motion state, and starting testing in a conventional power-on operation of 220V alternating voltage of equipment under a natural illumination condition.
Pollutants in FOX-7 synthetic simulation wastewater are mainly dimethyl sulfoxide and a small amount of mixed nitric-sulfuric acid, and COD indexes in the wastewater are detected according to GB 11914-89.
COD in the wastewater is detected regularly in the test process, and the detection data are shown in table 1 and figure 1.
TABLE 1 FOX-7 COD detection index change in synthetic simulated wastewater treatment
As can be seen from Table 1 and FIG. 1, the COD value in the raw water sample of the FOX-7 synthetic simulated wastewater is 1024.53mg/L, after 22 days of test, the COD value is reduced to 192.2mg/L and is maintained unchanged, and the COD index is reduced by 81.24%. The results show that the nano-diamond film has good degradation effect on dimethyl sulfoxide in FOX synthesis simulation wastewater after the test is started, and the COD index reduction amplitude is kept consistent along with the time extension until the final constant level is maintained and is kept unchanged. The nano diamond film has good treatment effect on the FOX synthetic wastewater.
Example 2
500mL of dimethyl sulfoxide was dissolved in 100L of tap water, and a small amount of nitric acid (0.01 wt%) and sulfuric acid (0.01 wt%) were added thereto and mixed uniformly to prepare FOX-7 synthesis-simulated wastewater. Immersing a workpiece containing the nano-diamond film in FOX-7 synthetic simulation wastewater, stirring to enable a water body to be in a motion state, and starting testing in a conventional power-on operation of 220V alternating voltage of equipment under a natural illumination condition.
Pollutants in FOX-7 synthetic simulation wastewater are mainly dimethyl sulfoxide and a small amount of mixed nitric-sulfuric acid, and COD indexes in the wastewater are detected according to GB 11914-89.
COD in the wastewater is detected regularly in the test process, and the detection data are shown in Table 2.
TABLE 2 FOX-7 COD detection index change in synthetic simulated wastewater treatment
As can be seen from Table 2, the COD value in the raw water sample of the FOX-7 synthetic simulated wastewater is 990.53mg/L, after 22 days of experiments, the COD value is reduced to 192.1mg/L and is maintained unchanged, and the COD index is reduced by 80.6%. The result shows that the diamond nano-film has good degradation effect on dimethyl sulfoxide in FOX synthesis simulation wastewater from the beginning of the test, and the COD index reduction amplitude is kept consistent with the time extension until the final constant level is maintained and is kept unchanged. The diamond nano-film has good treatment effect on the FOX synthetic wastewater.
Example 3
1000mL of dimethyl sulfoxide was dissolved in 200L of tap water, and a small amount of nitric acid (0.01 wt%) and sulfuric acid (0.01 wt%) were added thereto and mixed uniformly to prepare FOX-7 synthesis-simulated wastewater. Immersing a workpiece containing the nano-diamond film in FOX-7 synthetic simulation wastewater, stirring to enable a water body to be in a motion state, and starting testing in a conventional power-on operation of 220V alternating voltage of equipment under a natural illumination condition.
Pollutants in FOX-7 synthetic simulation wastewater are mainly dimethyl sulfoxide and a small amount of mixed nitric-sulfuric acid, and COD indexes in the wastewater are detected according to GB 11914-89.
COD in the wastewater is detected regularly in the test process, and the detection data are shown in Table 3.
TABLE 3 FOX-7 COD detection index change in synthetic simulated wastewater treatment
As can be seen from Table 3, the COD value in the raw water sample of the FOX-7 synthetic simulated wastewater is 1000.43mg/L, and after 22-day test, the COD value is reduced to 195.25mg/L and is maintained unchanged, and the COD index is reduced by 80.5%. The results show that the nano-diamond film has good degradation effect on dimethyl sulfoxide in FOX synthesis simulation wastewater after the test is started, and the COD index reduction amplitude is kept consistent along with the time extension until the final constant level is maintained and is kept unchanged. The nano diamond film has good treatment effect on the FOX synthetic wastewater.
The embodiments of the present invention have been described above. However, the present invention is not limited to the above embodiment. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (8)
1. A treatment method of FOX synthetic wastewater is characterized by comprising the following steps: the FOX synthetic wastewater is subjected to photocatalytic treatment by adopting a zero-dimensional carbon-based nano material under the conditions of illumination and electrification.
2. The treatment method according to claim 1, wherein the FOX synthesis wastewater contains dimethyl sulfoxide, and the volume percentage of the dimethyl sulfoxide is 0.2-0.8%.
3. The treatment method according to claim 2, wherein the FOX synthesis wastewater further contains nitric acid.
4. The treatment method according to claim 2 or 3, wherein the FOX synthesis wastewater further contains sulfuric acid.
5. The treatment method according to any one of claims 1 to 4, wherein the zero-dimensional carbon-based nanomaterial is selected from a nanodiamond material, preferably a nanodiamond thin film.
6. The processing method according to any one of claims 1 to 5, wherein the lighting conditions comprise: and (5) natural illumination.
7. The process of any one of claims 1 to 6, wherein the power-on conditions include: the current is 10-15A, the alternating voltage is 200-250V, and the power is continuously supplied.
8. The processing method according to any one of claims 1 to 7, wherein the processing procedure includes: the zero-dimensional carbon-based nano material is prepared into a film or coated on a carrier in a film form, and is immersed in FOX synthetic wastewater to enable a water body to be in a flowing state, and a photocatalytic reaction is carried out under the conditions of natural illumination and electrification.
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