CN110980919A - Method for degrading printing and dyeing wastewater by catalytic oxidation system based on persistent free radicals - Google Patents
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- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
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Abstract
The invention provides a method for degrading printing and dyeing wastewater by a catalytic oxidation system based on persistent free radicals, which comprises the steps of taking an iron complex as an active center, taking active carbon fibers rich in the persistent free radicals as a carrier, preparing the active carbon fibers of the iron-loaded complex by an impregnation method, and then adding persulfate, peroxymonosulfate or hydrogen peroxide to construct the catalytic oxidation system based on the persistent free radicals. The catalytic oxidation system can completely degrade pollutants after reacting for 5-30min under the irradiation of visible light or ultraviolet light. The method utilizes the persistent free radicals on the surface of the activated carbon fibers to activate persulfate, peroxymonosulfate or hydrogen peroxide to generate sulfate radicals and hydroxyl radicals with strong oxidizing property, has simple process, high catalytic activity, high utilization efficiency of the oxidant, high degradation rate and mild reaction conditions, and the environment-friendly catalytic oxidation system added into the dye wastewater does not cause secondary pollution to water, thereby having wide application prospect in wastewater treatment.
Description
Technical Field
The invention relates to a method for degrading printing and dyeing wastewater by a catalytic oxidation system based on persistent free radicals, belonging to the technical field of industrial wastewater treatment.
Background
As the first country of world textile printing and dyeing, dye wastewater becomes one of the main water pollution sources in China at present. The dye wastewater contains a large amount of dyes, has strong toxicity, great harm to human bodies, high chroma, easy damage to the appearance of water bodies, poor degradability and large total water volume, and is difficult to effectively treat by adopting a conventional method. Moreover, most dye wastewater contains organic matters with biotoxicity and 'three-cause' (carcinogenesis, teratogenesis and mutagenesis) properties, so the dye wastewater is always the focus and the difficulty of the treatment of industrial wastewater in China and is also one of the major problems to be solved by fishes in the field of water pollution control and treatment in China.
At present, although the Fenton technology and the Fenton-like technology have good effects on the aspect of treating dye wastewater, the defects of high treatment cost, high energy consumption, complex preparation, poor recycling performance and the like still exist. In order to find a technical method capable of efficiently degrading dye wastewater, relevant scholars at home and abroad research a plurality of new technologies such as advanced oxidation technology: under the reaction conditions of high temperature, high pressure, electricity, sound, light, catalyst, etc., active oxygen species with strong oxidizing property are produced to degrade high molecular organic matter into low molecular non-toxic matter.
How to generate a large amount of active oxygen species with high activity under relatively mild conditions has been a big problem in the field of environmental catalysis. Fahmy et al have shown that persistent free radicals can increase the production of reactive oxygen species. Although persistent free radicals cause oxidative stress in the organism, some deleterious effects are produced. However, if the method can change waste into valuable, and the strong capability of enhancing the generation of active oxygen species of persistent free radicals is applied to the aspect of wastewater treatment, the method has great application value. Unfortunately, few reports on persistent free radicals in the environment are currently seen. Therefore, the method for degrading the printing and dyeing wastewater by the catalytic oxidation system based on the persistent free radicals is developed, and has a great application prospect in the aspect of advanced treatment of industrial wastewater.
Disclosure of Invention
The invention aims to solve the technical problems of poor stability, metal pollution and the like in the existing organic wastewater treatment technology, and the defects of complex preparation process, low degradation efficiency of dye wastewater and the like.
In order to solve the technical problems, the invention provides a method for degrading printing and dyeing wastewater by using a catalytic oxidation system based on persistent free radicals, and the inventors have intensively studied and found that the catalytic oxidation system has an effect of efficiently degrading organic pollutants in dye wastewater.
The invention specifically adopts the technical scheme as follows:
a method for degrading printing and dyeing wastewater by a catalytic oxidation system based on persistent free radicals comprises the following specific steps: loading the iron complex onto the active carbon fiber rich in the persistent free radical by using the iron complex as an active center and the active carbon fiber rich in the persistent free radical as a carrier through an impregnation method, and forming a catalytic oxidation system by cooperating with an oxidant to degrade organic pollutants in the printing and dyeing wastewater through a reaction under illumination;
the iron complex is one or more of ferric citrate, ferric alginate and ferric oxalate, and the oxidant is one or more of persulfate, peroxymonosulfate or hydrogen peroxide.
Further, the ferric citrate is prepared from ferric salt and citrate according to the weight ratio of 1: (1-10) preparation by mixing iron salts including FeCl2、FeCl3、Fe(NO3)3、FeSO4、Fe2(SO4)3And citrate comprises sodium citrate, potassium citrate, calcium citrate, or magnesium citrate.
Further, the ferric alginate is prepared from ferric salt and alginate according to the weight ratio of 1: (1-10) preparation by mixing iron salts including FeCl2、FeCl3、Fe(NO3)3、FeSO4、Fe2(SO4)3AOr the combination of two or more of them, and the alginate is sodium alginate, potassium alginate, calcium alginate or magnesium alginate.
Further, the ferric oxalate is prepared from ferric salt and oxalate according to the ratio of 1: (1-8) in a mass ratio, iron salt including FeCl2、FeCl3、Fe(NO3)3、FeSO4、Fe2(SO4)3The oxalate is sodium oxalate, potassium oxalate, calcium oxalate or magnesium oxalate.
Further, the activated carbon fiber is in a felt form, and is soaked after being cut, and the size of the cut block is as follows: the length and width are 1-5cm, the thickness is 0.1-10mm, and the weight of the single block is 0.05-0.2 g.
Furthermore, in the impregnation method, the concentration of the iron complex used for impregnation is 0.04-0.5mol/L, the impregnation temperature is 20-60 ℃, the impregnation time is 1-24h, and the iron complex in the impregnation liquid is completely loaded on the activated carbon fiber.
Further, in the oxidizing agent, the persulfate is one or more of sodium persulfate, potassium persulfate, or ammonium persulfate, and the peroxymonosulfate is one or more of sodium peroxymonosulfate, potassium peroxymonosulfate, or ammonium peroxymonosulfate.
Furthermore, in the catalytic oxidation system, the concentration of the oxidant is 0.01-100mmol/L, the degradation reaction temperature is controlled at 10-80 ℃, and the degradation reaction time is 5-30 min.
Further, the illumination is ultraviolet illumination or visible illumination, the illumination intensity is 200-500W, and the illumination time is 5-60 min.
Further, the organic pollutants in the printing and dyeing wastewater are one or more of reactive dyes, acid dyes, basic dyes, disperse dyes, azo dyes, sulfur dyes and direct dyes, and the concentration of the organic pollutants is 0.02-50 g/L.
The invention has the advantages that:
(1) the iron complex of the catalytic oxidation system is synthesized by one step by a hydrothermal method from low-cost natural environment-friendly alginic acid, citric acid or oxalic acid and iron elements widely existing in the nature, so that the cost is low, the catalytic oxidation system is green and environment-friendly, and the preparation process is simple and convenient;
(2) the reaction for degrading the dye wastewater can be carried out under visible light, and the application of the traditional photocatalyst in ultraviolet light is broken through;
(3) the catalytic oxidation system can completely degrade dyes within 20min under visible light, and has extremely high degradation efficiency;
(4) after continuous reaction for 6 periods, the catalytic oxidation system can still reach 94 percent of degradation rate within 20min, and the excellent cyclability and the longer service life of the catalytic oxidation system are reflected;
(5) the catalytic oxidation system has good degradation effect on typical dyes such as reactive dyes, acid dyes, basic dyes, direct dyes and the like, and experiments show that the degradation rate of the dyes within 20min is up to more than 95%, so that the catalytic oxidation system has wide applicability and universal applicability;
(6) experiments show that the degradation rate of the catalytic oxidation system to the dye is up to more than 95% under the condition that the pH value is 2-10. The catalytic oxidation system is suitable for both acid environment and alkaline environment, and has wide pH applicability;
(7) the research shows that the active carbon fiber of the catalytic oxidation system can provide persistent free radicals, has the obvious advantage of long service life and has a half-life period of hours or even days, and the active oxygen species OH is only 10-9And s. In addition, the persistent free radical can also be used as an electron donor to provide free electrons, so that the oxidation-reduction reaction process which is important in environmental catalysis is accelerated. Therefore, the system has wide application prospect in the field of environmental catalysis. At the same time, carbonaceous materials play an important role in the field of environmental science, having attractive physical and chemical properties that may confer potential applications for persistent free-radical environmental catalysis.
Drawings
FIG. 1 is a diagram of the degradation mechanism of a catalytic oxidation system based on persistent free radicals to acid red 1 dye;
FIG. 2 is a graph showing the effect of a catalytic oxidation system based on persistent free radicals on the removal of acid Red 1 dye;
FIG. 3 is a graph showing the effect of a catalytic oxidation system based on persistent free radicals on the removal of reactive bright red X-3B dye;
FIG. 4 is a graph of the effect of a catalytic oxidation system based on persistent free radicals on the removal of methylene blue dye;
FIG. 5 is a graph showing the effect of a catalytic oxidation system based on persistent free radicals on the removal of basic green dye;
FIG. 6 is a schematic representation of the reusability of a catalytic oxidation system based on persistent free radicals.
Detailed Description
The method for degrading printing and dyeing wastewater by using the catalytic oxidation system based on the persistent free radicals in the invention is further described by combining the examples.
In the following examples, the activated carbon fibers used were pretreated with an acid pretreatment in advance by the following method: activated Carbon Fibers (ACF) in the form of felt were cut into small pieces having a length × width of 1cm × 1cm and a thickness of about 1cm, and the weight of each piece was about 0.1 g. Then immersing the cut activated carbon fiber in 3mol/L nitric acid, mixing uniformly, reacting for 6 hours at 30 ℃, washing with distilled water for multiple times, and drying at 40 ℃. Research shows that the activated carbon fiber can provide persistent free radicals, and has the obvious advantage of long service life, and the short half life is exceeded by hours or even days.
Next, tests of the following examples were carried out using the activated carbon fiber.
Example 1
0.1g of sodium alginate and 0.1g of ferric chloride are dissolved in 200mL of distilled water and stirred to be gelatinous, thus obtaining the ferric alginate solution. And soaking the activated carbon fiber into the ferric alginate solution for 24 hours, controlling the water temperature to be kept at 30 ℃, and preparing the activated carbon fiber loaded with the ferric alginate by an impregnation method. Respectively adding activated carbon fiber loaded with ferric alginate and potassium monopersulfate into acid red 1 dye wastewater with the concentration of 0.1g/L, wherein the weight of the activated carbon fiber is 0.1g, the concentration of the potassium monopersulfate is 0.05mmol/L, reacting for 20min under visible light at the temperature of 10 ℃, and the removal rate of the acid red 1 dye can reach more than 98%. The test results refer to fig. 2.
Example 2
Respectively adding activated carbon fiber loaded with ferric alginate and potassium monopersulfate into acid red 1 dye wastewater with the concentration of 20g/L, wherein the weight of the activated carbon fiber is 0.1g, the concentration of the potassium monopersulfate is 50mmol/L, the other conditions are the same as those of the example 1, reacting for 30min under visible light at the temperature of 60 ℃, and the removal rate of the acid red 1 dye can reach more than 98%.
Examples 3 to 4
The iron complex of ferric citrate and ferric oxalate is used to replace the ferric alginate in the example 1, the other conditions are the same as those in the example 1, and the removal rate of the acid red 1 dye can reach more than 97%.
Examples 5 to 9
The potassium peroxymonosulfate in the embodiment 1 is replaced by one of sodium persulfate, potassium persulfate, ammonium persulfate, sodium peroxymonosulfate or ammonium peroxymonosulfate in the oxidizing agent, other conditions are consistent with those of the embodiment 1, and the removal rate of the acid red 1 dye can reach more than 97%.
Example 10
0.1g of sodium alginate and 0.1g of ferric chloride are dissolved in 200mL of distilled water and stirred to be gelatinous, thus obtaining the ferric alginate solution. And soaking the activated carbon fiber into the ferric alginate solution for 24 hours, controlling the water temperature to be kept at 30 ℃, and preparing the activated carbon fiber loaded with the ferric alginate by an impregnation method. Respectively adding activated carbon fiber loaded with ferric alginate and sodium persulfate into the activated brilliant red X-3B dye wastewater with the concentration of 0.02g/L, stirring, wherein the weight of the activated carbon fiber is 0.05g, the concentration of the sodium persulfate is 0.01mmol/L, reacting for 20min under visible light at the temperature of 30 ℃, and the removal rate of the activated brilliant red X-3B dye can reach more than 96%. The test results refer to fig. 3.
Examples 11 to 12
The ferric alginate in the example 10 is replaced by ferric citrate and ferric oxalate in the iron complex, other conditions are the same as those in the example 10, and the removal rate of the reactive brilliant red X-3B dye can reach more than 96%.
Examples 13 to 17
Respectively replacing sodium persulfate in the embodiment 10 by one of potassium persulfate, ammonium persulfate, sodium peroxymonosulfate, potassium peroxymonosulfate or ammonium peroxymonosulfate in the oxidant, wherein other conditions are consistent with those of the embodiment 10, and the removal rate of the reactive brilliant red X-3B dye can reach more than 96%.
Example 18
Dissolving 1g of sodium citrate and 0.1g of ferric chloride in 200mL of distilled water, and stirring to form a gel, thereby obtaining a ferric citrate solution. And soaking the activated carbon fiber into a ferric citrate solution for 24 hours, controlling the water temperature to be kept at 30 ℃, and preparing the ferric citrate loaded activated carbon fiber by an impregnation method. Respectively adding activated carbon fiber loaded with ferric citrate and potassium peroxymonosulfate into methylene blue dye wastewater with the concentration of 50g/L, stirring, wherein the weight of the activated carbon fiber is 0.1g, the concentration of the potassium peroxymonosulfate is 100mmol/L, reacting for 20min under visible light at the temperature of 60 ℃, and the removal rate of the methylene blue dye can reach more than 99%. The test results refer to fig. 4.
Examples 19 to 20
The other conditions are the same as those of example 18 except that ferric citrate in example 18 is replaced by ferric alginate and ferric oxalate in the iron complex, and the removal rate of the methylene blue dye can reach more than 98%.
Examples 21 to 25
The potassium peroxymonosulfate in the example 18 is replaced by one of sodium persulfate, potassium persulfate, ammonium persulfate, sodium peroxymonosulfate or ammonium peroxymonosulfate in the oxidizing agent respectively, other conditions are consistent with those of the example 18, and the removal rate of the methylene blue dye can reach more than 99%.
Example 26
0.2g of potassium oxalate and 0.1g of ferric chloride are dissolved in 100mL of distilled water and stirred to be gelatinous, thus obtaining the ferric oxalate solution. And soaking the activated carbon fiber into an iron oxalate solution for 24 hours, controlling the water temperature to be kept at 30 ℃, and preparing the activated carbon fiber loaded with the iron oxalate by an impregnation method. Respectively adding activated carbon fiber loaded with ferric oxalate and sodium peroxymonosulfate into alkaline green dye wastewater with the concentration of 1g/L, stirring, wherein the weight of the activated carbon fiber is 0.1g, the concentration of the sodium peroxymonosulfate is 50mmol/L, reacting for 20min under visible light at the temperature of 10 ℃, and the removal rate of the alkaline green dye can reach more than 99%. The test results refer to fig. 5.
Example 27
The iron alginate loaded activated carbon fiber after the reaction of example 1 was taken out and reused, and the reaction conditions for each use were the same as those of example 1. When the fiber is used for carrying out catalytic oxidation reaction for six times, the catalytic oxidation system still has a dye removal rate as high as 94%. The test results refer to fig. 6.
Example 28
Multiple treatment groups were set up and the catalytic degradation of acid red 1 dye was carried out as in example 1, but the pH of the acid red 1 dye wastewater was adjusted to 2, 3, 4, …,10, respectively, with the remaining parameters being in accordance with example 1. The results show that the catalytic oxidation system has a removal rate of over 96 percent, but the degradation is faster under the acidic condition and slower under the alkaline condition. Therefore, the carbon fiber modified based on the ferric alginate has low requirements on reaction pH, and can efficiently degrade the dye acid red 1 in the printing and dyeing wastewater within a wide pH range of 2-10.
Example 29
Multiple treatment groups were set up and the catalytic degradation of acid red 1 dye was carried out as in example 3, but the pH of the acid red 1 dye wastewater was adjusted to 2, 3, 4, …,10, respectively, with the remaining parameters being in accordance with example 3. The results show that the catalytic oxidation system has a removal rate of over 95 percent, but the degradation is faster under the acidic condition and slower under the alkaline condition. Therefore, the carbon fiber modified based on ferric citrate and ferric oxalate has low requirement on reaction pH, and can efficiently degrade acid red 1 dye in printing and dyeing wastewater in a wide pH range of 2-10.
The above description is only a part of the embodiments of the present invention, and the protection scope of the present invention is not limited to the above embodiments, and does not represent all technical solutions under the concept of the present invention. It should be noted that, for a person skilled in the art, several modifications and additions can be made without departing from the method of the invention, which should also be considered as a protection scope of the invention.
Claims (10)
1. A method for degrading printing and dyeing wastewater by a catalytic oxidation system based on persistent free radicals is characterized by comprising the following steps: loading the iron complex onto the active carbon fiber rich in the persistent free radical by using the iron complex as an active center and the active carbon fiber rich in the persistent free radical as a carrier through an impregnation method, and forming a catalytic oxidation system by cooperating with an oxidant to degrade organic pollutants in the printing and dyeing wastewater through a reaction under illumination;
the iron complex is one or more of ferric citrate, ferric alginate and ferric oxalate, and the oxidant is one or more of persulfate, peroxymonosulfate or hydrogen peroxide.
2. The method for oxidative degradation of dye wastewater based on persistent radical-activated persulfate as claimed in claim 1, wherein: the ferric citrate is prepared from ferric salt and citrate according to the weight ratio of 1: (1-10) preparation by mixing iron salts including FeCl2、FeCl3、Fe(NO3)3、FeSO4、Fe2(SO4)3And citrate comprises sodium citrate, potassium citrate, calcium citrate, or magnesium citrate.
3. The method for oxidative degradation of dye wastewater based on persistent radical-activated persulfate as claimed in claim 1, wherein: the iron alginate is prepared from ferric salt and alginate according to the proportion of 1: (1-10) preparation by mixing iron salts including FeCl2、FeCl3、Fe(NO3)3、FeSO4、Fe2(SO4)3The alginate is sodium alginate, potassium alginate, calcium alginate or magnesium alginate.
4. The method for oxidative degradation of dye wastewater based on persistent radical-activated persulfate as claimed in claim 1, wherein: the ferric oxalate is prepared from ferric salt and oxalate according to the proportion of 1: (1-8) in a mass ratio, iron salt including FeCl2、FeCl3、Fe(NO3)3、FeSO4、Fe2(SO4)3The oxalate is sodium oxalate, potassium oxalate, calcium oxalate or magnesium oxalate.
5. The method for degrading printing and dyeing wastewater based on the catalytic oxidation system of the persistent free radicals as claimed in claim 1, wherein the catalytic oxidation system comprises: the activated carbon fiber adopts a felt form, and is soaked after being cut, and the size of the cut block body is as follows: the length and width are 1-5cm, the thickness is 0.1-10mm, and the weight of the single block is 0.05-0.2 g.
6. The method for degrading printing and dyeing wastewater based on the catalytic oxidation system of the persistent free radicals as claimed in claim 1, wherein the catalytic oxidation system comprises: in the impregnation method, the concentration of the iron complex used for impregnation is 0.04-0.5mol/L, the impregnation temperature is 20-60 ℃, the impregnation time is 1-24h, and the iron complex in the impregnation liquid is completely loaded on the activated carbon fiber.
7. The method for degrading printing and dyeing wastewater based on the catalytic oxidation system of the persistent free radicals as claimed in claim 1, wherein the catalytic oxidation system comprises: in the oxidant, the persulfate is one or more of sodium persulfate, potassium persulfate or ammonium persulfate, and the peroxymonosulfate is one or more of sodium peroxymonosulfate, potassium peroxymonosulfate or ammonium peroxymonosulfate.
8. The method for degrading printing and dyeing wastewater based on the catalytic oxidation system of the persistent free radicals as claimed in claim 1, wherein the catalytic oxidation system comprises: in the catalytic oxidation system, the concentration of the oxidant is 0.01-100mmol/L, the degradation reaction temperature is controlled at 10-80 ℃, and the degradation reaction time is 5-30 min.
9. The method for oxidative degradation of dye wastewater based on persistent radical-activated persulfate as claimed in claim 1, wherein: the illumination is ultraviolet illumination or visible illumination, the illumination intensity is 200-.
10. The method for degrading printing and dyeing wastewater based on the catalytic oxidation system of the persistent free radicals as claimed in claim 1, wherein the catalytic oxidation system comprises: the organic pollutants in the printing and dyeing wastewater are one or more of reactive dyes, acid dyes, basic dyes, disperse dyes, azo dyes, sulfur dyes and direct dyes, and the concentration of the organic pollutants is 0.02-50 g/L.
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| CN115974258A (en) * | 2023-01-10 | 2023-04-18 | 安徽工业大学 | Method for removing humic acid in water body |
| CN115974258B (en) * | 2023-01-10 | 2023-10-17 | 安徽工业大学 | Method for removing humic acid in water body |
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Application publication date: 20200410 |