CN110575847B - Polymer non-covalent modified carbon nano tube and application thereof - Google Patents

Polymer non-covalent modified carbon nano tube and application thereof Download PDF

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CN110575847B
CN110575847B CN201910735717.3A CN201910735717A CN110575847B CN 110575847 B CN110575847 B CN 110575847B CN 201910735717 A CN201910735717 A CN 201910735717A CN 110575847 B CN110575847 B CN 110575847B
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欧阳钢锋
王俊慧
付琦
郁家星
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Sun Yat Sen University
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    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/72—Treatment of water, waste water, or sewage by oxidation
    • C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
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    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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Abstract

The invention discloses a polymer non-covalent modified carbon nano tube and application thereof. The polymer non-covalent modified carbon nanotube is prepared by the following steps: dispersing carbon nano tubes and a polymer aqueous solution in water, performing ultrasonic treatment, stirring, centrifuging, washing and drying to obtain the carbon polymer non-covalent modified carbon nano tubes; the polymer aqueous solution is a polyethyleneimine aqueous solution or a polydiallyldimethylammonium chloride aqueous solution. The polymer non-covalent modified carbon nano tube can rapidly and efficiently catalyze and activate persulfate to degrade organic pollutants in a mode of mediating electron transfer at normal temperature, has a wide applicable pH range and is slightly interfered by natural organic matters in the environment; the method for degrading organic pollutants in water has the advantages of low cost, high treatment efficiency at normal temperature, mild reaction conditions, simple operation, low equipment requirement, economy and high efficiency, and the organic matters in natural water have little interference on the treatment effect, thereby having wide market prospect.

Description

Polymer non-covalent modified carbon nano tube and application thereof
Technical Field
The invention relates to the technical field of environmental pollution treatment, relates to an advanced oxidation technology of organic matters in water, and more particularly relates to a polymer non-covalent modified carbon nanotube and application thereof.
Background
At present, the treatment methods of organic polluted wastewater mainly comprise three major types, namely a physical adsorption method, a biological treatment method and an advanced oxidation method. Physical adsorption is one of the most common treatment technologies in sewage treatment at present, but the adsorption only can reduce the concentration of pollutants in a water body and cannot completely remove the pollutants, and the pollutants can enter the water environment again. The traditional biological treatment technology has an unsatisfactory treatment effect on waste water containing organic pollutants with high concentration and stable chemical structure, such as pesticides, papermaking water, printing and dyeing waste water and the like. The organic pollutants are high in concentration, high in toxicity, complex in components, mostly contain stable aromatic structures which are difficult to degrade, poor in biodegradability and high in treatment difficulty. The advanced oxidation technology has high oxidation rate of pollutants, simple and convenient operation, easy control and no secondary pollution, thereby having great application prospect.
Traditional advanced oxidation technologies include three major classes of fenton, electrocatalysis, and photocatalysis. The Fenton technique has a high oxidation rate of pollutants, but requires harsh pH conditions and the addition of a large amount of reagent. The electric catalysis can thoroughly decompose and mineralize the pollutants in the water into nontoxic CO2And H2O, but the energy consumption is higher. Although the photocatalytic oxidation technology has the advantages of energy conservation, mild reaction conditions and no secondary pollution, the photocatalytic oxidation technology is only limited to laboratory research at present and cannot be put into practical application.
The persulfate activation technology based on the sulfuric acid free radical for deeply treating the organic pollutants in the wastewater is a novel advanced oxidation technology developed in recent years. In light, heat and Fe2+、Co2+Under the activation of transition metal ions, persulfate can generate sulfate radicals, and most of organic pollutants are efficiently oxidized and degraded. However, the catalytic activity of the catalyst based on the free radical mechanism is greatly inhibited under the condition of environmental interference.
In recent years, researchers find that carbon materials such as carbon nanotubes, graphene and diamond can activate persulfate to degrade pollutants through a non-free radical mechanism by taking the carbon materials as catalysts, can resist the interference of organic matters in the environment, and realize the selective oxidative degradation of target pollutants. In order to improve the catalytic activity of the carbon material, N doping is a very effective way, but the modification way needs to be realized under high temperature conditions, and the equipment conditions are harsh.
Therefore, a simple N-doping method is provided, the N-doped carbon nano tube is prepared, the N-doped carbon nano tube is used for efficiently catalyzing persulfate, and the N-doped carbon nano tube has a great application prospect in treating organic pollutants in wastewater.
Disclosure of Invention
The invention aims to provide a polymer non-covalent modified carbon nanotube. According to the invention, the polymer is modified on the carbon nano tube through non-covalent acting force, the preparation method is simple, the N content in the modified carbon nano tube is obviously increased, the prepared N-doped carbon nano tube can rapidly and efficiently catalyze and activate persulfate to degrade organic pollutants in a mode of mediating electron transfer at normal temperature, the pH range is wide, the good treatment effect can be achieved in acidic, neutral and weakly alkaline water, and the interference of natural organic matters in the environment is very small.
The invention also aims to provide application of the polymer to non-covalent modification of the carbon nanotube. The method for degrading organic pollutants in wastewater by using the polymer non-covalent modified carbon nano tube has the advantages of low cost, high treatment efficiency at normal temperature, simple operation and great potential in the technical field of organic wastewater treatment.
The above object of the present invention is achieved by the following scheme:
a polymer non-covalent modified carbon nanotube is prepared by the following steps: dispersing a carbon nano tube and a polymer aqueous solution in water, performing ultrasonic treatment, stirring, centrifuging, washing and drying to obtain the polymer non-covalent modified carbon nano tube;
the polymer aqueous solution is a polyethyleneimine aqueous solution or a polydiallyldimethylammonium chloride aqueous solution.
Preferably, the mass ratio of the carbon nanotubes to the polymer is: 100: 0.5-40.
Preferably, the mass ratio of the carbon nanotubes to the polymer is: 100: 1-10.
Preferably, the concentration of the polymer in the aqueous solution is 0.5-20 g/L.
Preferably, the carbon nanotubes are single-walled or multi-walled carbon nanotubes.
Preferably, the ultrasonic time is 2-10 h; stirring for 5-24 h; the drying is vacuum drying at 70-100 ℃.
The invention also protects the application of the polymer non-covalent modified carbon nano tube as a catalyst for organic pollutants in water.
Preferably, the polymer non-covalently modified carbon nanotubes catalyze persulfate to degrade organic pollutants in water.
Preferably, the specific process is as follows: at normal temperature, persulfate and the polymer modified carbon nano tube are added into water containing organic pollutants, the polymer modified carbon nano tube is used as a catalyst, and the persulfate is catalyzed to degrade the organic pollutants, so that the organic pollutants in the water can be removed.
Preferably, the persulfate is potassium monopersulfate, sodium monopersulfate, amine monopersulfate, potassium hydrogen peroxodisulfate, or sodium hydrogen peroxodisulfate.
Preferably, the mass concentration of the polymer non-covalent modified carbon nano tube in water is 0.1-2.0 g/L.
Preferably, the organic contaminant is bisphenol A, phenol, 4-chlorophenol, methyl orange, methyl red, propranolol, or sulfamethoxazole.
Compared with the prior art, the invention has the following beneficial effects:
according to the invention, the polymer is modified on the carbon nano tube through non-covalent acting force, the preparation method is simple, the N content in the modified carbon nano tube is obviously increased, the prepared N-doped carbon nano tube can rapidly and efficiently catalyze and activate persulfate to degrade organic pollutants in a mode of mediating electron transfer at normal temperature, the pH range is wide, the good treatment effect can be achieved in acidic, neutral and weakly alkaline water, and the interference of natural organic matters in the environment is very small.
The method for degrading organic pollutants in wastewater by using the polymer non-covalent modified carbon nano tube has the advantages of low cost, high treatment efficiency at normal temperature, mild reaction conditions, simplicity in operation, low requirement on equipment, economy and high efficiency, and has wide market prospect because the organic matters in natural water have little interference on treatment effect.
Drawings
FIG. 1 is a graph showing the effect of different catalysts on the treatment of bisphenol A in simulated wastewater (potassium peroxodisulfate is used as the oxidizing agent).
FIG. 2 is a graph showing the effect of different catalysts on the treatment of bisphenol A in simulated wastewater (potassium hydrogen peroxymonosulfate is used as the oxidizing agent).
FIG. 3 is a schematic diagram of the effect of activated potassium persulfate degradation simulation of bisphenol A in wastewater under different pH conditions using PEI-MWCNT as catalyst.
FIG. 4 is a schematic diagram showing the effect of degrading bisphenol A in simulated wastewater under different potassium persulfate dosages by using PEI-MWCNT as a catalyst.
FIG. 5 is a schematic diagram of the effect of degrading bisphenol A in simulated wastewater under different anion interference conditions by using PEI-MWCNT as a catalyst.
FIG. 6 is a schematic diagram showing the effect of natural organic substances on the degradation of bisphenol A in simulated wastewater by using PEI-MWCNT as a catalyst.
Detailed Description
The present invention is further described in detail below with reference to specific examples, which are provided for illustration only and are not intended to limit the scope of the present invention. The test methods used in the following examples are all conventional methods unless otherwise specified; the materials, reagents and the like used are, unless otherwise specified, commercially available reagents and materials.
Example 1
A polymer non-covalent modified carbon nano tube is prepared by the following specific steps:
dispersing 50mg of multi-walled carbon nanotubes and 5mL of polyethyleneimine water solution with the concentration of 0.1g/L into 50mL of water, performing ultrasonic treatment for 2h (40Hz, 35 ℃), stirring overnight, centrifuging, washing with water and ethanol for three times respectively, and finally performing vacuum drying at 70-100 ℃ to obtain the polyethyleneimine non-covalent modified multi-walled carbon nanotubes.
The multi-walled carbon nanotube is replaced by a single-walled carbon nanotube, and the polyethyleneimine non-covalent modified single-walled carbon nanotube can be prepared.
TABLE 1 elemental analysis results of multiwall carbon nanotubes before and after modification
Material C(％) N(％) H(％)
Multiwalled carbon nanotube 92.87 0.27 1.59
Polyethyleneimine non-covalent modified multi-walled carbon nanotube 89.82 2.65 1.47
Example 2
The specific preparation process of the polymer non-covalent modified carbon nanotube is the same as that in example 1, except that the polymer is poly (diallyldimethylammonium chloride).
Example 3 application test
The polymer non-covalent modified carbon nano tube prepared in the embodiment 1 or the embodiment 2 is used as a catalyst to treat bisphenol A in wastewater, and the specific treatment process is as follows: putting the polymer non-covalent modified carbon nano tube (catalyst) and persulfate (oxidant) into the wastewater, stirring, detecting the content of the bisphenol A in the water after a certain time, and comparing the content with the content of the bisphenol A in the water before treatment to calculate the degradation rate of the bisphenol A. Meanwhile, carbon nanotubes without polymer modification are used as a control.
Specifically, the catalyst and the oxidant used, and the degradation results are shown in table 1, wherein the test temperature is 25 ℃ and the system pH is 7.
In the following table, MWCNT is multi-walled carbon nanotube, PDDA-MWCNT is poly diallyldimethylammonium chloride non-covalent modification multi-walled carbon nanotube, PEI-MWCNT is polyethyleneimine non-covalent modification multi-walled carbon nanotube.
TABLE 1 results of various catalysts, oxidants and their degradation of bisphenol A
Figure BDA0002162097860000041
Figure BDA0002162097860000051
As can be seen from table 1 and fig. 1, the PDDA-MWCNT and PEI-MWCNT can significantly catalyze potassium disulfate to oxidize bisphenol a, and have better and faster degradation effect on bisphenol a in wastewater compared to unmodified carbon nanotubes in treatments 1 to 3.
From treatments 1 to 6, it is known that the oxidation effect of the PDDA-MWCNT or PEI-MWCNT on bisphenol A is significantly better than that of the PDDA-MWCNT or PEI-MWCNT when the PDDA-MWCNT or PEI-MWCNT is combined with potassium disulfate. The results are shown in FIGS. 1 and 2.
From treatments 7 to 10, it is known that PEI-MWCNT can rapidly catalyze potassium disulfate to effectively degrade bisphenol A under acidic, neutral and weakly alkaline conditions. The results are shown in FIG. 3.
From treatments 12 to 15, it was found that bisphenol A was effectively degraded when the concentration of the oxidizing agent potassium disulfate in the system was higher than 0.75 mM. The results are shown in FIG. 4.
The results of the effect of the inorganic anions present in the water on the degradation of organic contaminants in the water are shown in Table 2.
TABLE 2 degradation results of bisphenol A by catalysts and oxidants in the presence of anions
Figure BDA0002162097860000061
In all of treatments 17 to 19, the concentration of the anion was 500mM, and from these 4 treatments, it was found that PDDA-MWCNT or PEI-MWCNT, when used in combination with potassium dithiolate, had a good degradation effect on bisphenol A in the presence of the anion. The results are shown in FIG. 5.
The results of the effect of natural organic substances present in water on the degradation of organic contaminants in water are shown in table 3 and fig. 6.
TABLE 3 degradation results of bisphenol A by catalysts and oxidants in the presence of natural organic matter
Figure BDA0002162097860000062
The degradation of different kinds of organic pollutants in water is shown in Table 4.
Table 4 degradation results of catalyst and oxidant for different contaminants
Figure BDA0002162097860000063
The experimental results show that the polymer non-covalent modified carbon nano tube prepared by the invention can rapidly and efficiently catalyze and activate persulfate to degrade organic pollutants, has a wide pH range, can achieve good treatment effects in acidic, neutral and weakly alkaline water, is slightly interfered by natural organic matters in the environment, and simultaneously has good degradation effect on various organic pollutants.
It should be finally noted that the above examples are only intended to illustrate the technical solutions of the present invention, and not to limit the scope of the present invention, and that other variations and modifications based on the above description and thought may be made by those skilled in the art, and that all embodiments need not be exhaustive. Any modification, equivalent replacement, and improvement made within the spirit and principle of the present invention should be included in the protection scope of the claims of the present invention.

Claims (7)

1. The application of the polymer non-covalent modified carbon nano tube in catalyzing persulfate to degrade organic pollutants in water is characterized in that the polymer non-covalent modified carbon nano tube is prepared by the following steps: dispersing a carbon nano tube and a polymer aqueous solution in water, performing ultrasonic treatment, stirring, centrifuging, washing and drying to obtain the polymer non-covalent modified carbon nano tube;
the polymer aqueous solution is a polyethyleneimine aqueous solution or a polydiallyldimethylammonium chloride aqueous solution; the ultrasonic time is 2-10 h; stirring for 5-24 h; the drying is vacuum drying at 70-100 ℃.
2. The application of the polymer non-covalently modified carbon nanotube for catalyzing persulfate to degrade organic pollutants in water according to claim 1, wherein the mass ratio of the carbon nanotube to the polymer is as follows: 100: 0.5-40.
3. The application of the polymer non-covalently modified carbon nanotube for catalyzing persulfate to degrade organic pollutants in water according to claim 2, wherein the mass ratio of the carbon nanotube to the polymer is as follows: 100: 1-10.
4. The application of the polymer non-covalently modified carbon nanotube for catalyzing persulfate to degrade organic pollutants in water according to claim 1, wherein the concentration of the polymer in an aqueous solution is 0.5-20 g/L.
5. The use of the polymer non-covalently modified carbon nanotubes to catalyze persulfate degradation of organic pollutants in water according to claim 1, wherein the carbon nanotubes are single-walled or multi-walled carbon nanotubes.
6. The application of the polymer non-covalently modified carbon nanotube for catalyzing persulfate to degrade organic pollutants in water according to claim 1 is characterized by comprising the following specific steps: at normal temperature, persulfate and the polymer modified carbon nano tube are added into water containing organic pollutants, the polymer modified carbon nano tube is used as a catalyst, and the persulfate is catalyzed to degrade the organic pollutants, so that the organic pollutants in the water can be removed.
7. The use of the polymer non-covalently modified carbon nanotubes to catalyze persulfate degradation of organic pollutants in water according to claim 6, wherein the persulfate is potassium monopersulfate, sodium monopersulfate, amine monopersulfate, potassium hydrogen peroxodisulfate, or sodium hydrogen peroxodisulfate;
the mass concentration of the polymer non-covalent modified carbon nano tube in water is 0.1-2.0 g/L.
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