CN110028137B - Electro-adsorption material for removing low-valent ions and COD in water body and application - Google Patents
Electro-adsorption material for removing low-valent ions and COD in water body and application Download PDFInfo
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Abstract
The invention discloses an electro-adsorption material for removing low-valence ions and COD in a water body and application thereof. The method takes low-grade molybdenum-containing sulfide ore, molybdenite and molybdenite tailings as precursors 1, takes graphite, lignite and weathered coal as precursors 2, and forms ultrafine nano-particle MoO by oxidizing, roasting and volatilizing the precursors 1 at high temperature3(ii) a Uniformly mixing the precursor 2, roasting, and carrying out superfine grinding to obtain an active substance carrier; using vapor deposition to form ultrafine nano-particle MoO3Uniformly loading the active substance carrier with the active substance carrier to prepare a composite material containing the active substance and the conductive substance; then adding a binder, and molding to prepare the electro-adsorption material; the electro-adsorption material is used for adsorbing and purifying water containing low-valence ions and high COD, the removal rate of the low-valence ions reaches 95%, and the removal rate of the COD reaches more than 98%.
Description
Technical Field
The invention belongs to the technical field of low-quality mineral products, solid waste resource utilization and waste water treatment, and particularly relates to an electro-adsorption material for removing low-valent ions and COD in a water body and application thereof.
Background
With the rapid development of chemical industry in China, various novel chemical products are applied to various industries, particularly in the heavy pollution industries such as medicine, chemical industry, electroplating, printing and dyeing and the like, and the increasingly serious environmental pollution problem is brought while the product quality and quality are improved, which is mainly shown in that: high salinity, high concentration of organic pollutants, stable structure, poor biodegradability, difficult realization of standard discharge of the conventional process and high treatment cost. The water body rich in low-valence ions and COD has serious inhibition and toxic effects on the growth of microorganisms; the higher the COD content in the water body is, the aquatic organisms can be anoxic and dead, and the serious pollution to the water quality is caused. Some of the organic substances with strong toxicity harm plants, animals and even human beings along with the extension of the biological chain. Aiming at the current situation, a great deal of research is carried out on the aspects of removing low-valence ions and COD in water at home and abroad. For example, Zhang Feng in "culture method of COD degradative bacteria" (CN 106957800A) proposed that the culture of COD degradative bacteria using nutrient agar medium can effectively improve the degradation rate of COD, but the culture process of the degradative bacteria is complicated, the conditions are difficult to control, and the degradation period is long. In the 'high-salt high-COD wastewater treatment system and process' (CN 109205872A) in the chapter, etc., the combination of several units of filtration-electrodialysis-coagulating sedimentation-evaporation concentration crystallization-degradation is proposed to realize the extraction of salt and the degradation of COD in the water body, but the process is more complex. The gross strength is in 'a treatment method of high-salt high-COD wastewater' (CN 109111043A), the combination of operation units such as air flotation, coarse filtration, extraction, enzymolysis and the like is provided for the high-salt high-COD wastewater, and the degradation of COD and Mg are realized2+、Ca2+、Zn2+The chlorine salt is removed, but the process and the conditions are more complicated.
In conclusion, the problems of complex process, high energy consumption, complex equipment and the like mainly exist in the treatment of low-valence ions and COD in the water body at present. In order to solve the problems, scholars develop an electro-adsorption technology for treating wastewater, and the electro-adsorption method has the advantages of low energy consumption, low cost, simple equipment and the like, but is not suitable for effectively removing low-valence ions and COD (chemical oxygen demand) at the same time. For example, Wanghui et al in 'application of ion selective multiple modified composite electrode material, preparation method and electro-adsorption desalination' (CN 108911058A)2The felt material is subjected to combined multiple basic modification, and the modified felt material and the metal material are subjected to composite adhesion by utilizing conductive silver adhesive to prepare the multiple modified electrode material. When the material is used for desalting treatment of salt-containing industrial wastewater with high hardness and complex components, the action effect has the characteristic of singleness, and the treatment effect on a mixed solution containing COD and low-valent ions is poor. Therefore, aiming at the water body rich in low-valence ions and high COD, the novel electro-adsorption material prepared by taking mineral resources as raw materials is provided, so that the material utilization of the traditional mineral resources is realized, and the purification of water body pollutants is also realized.
Disclosure of Invention
Aiming at the problems of complex process, high energy consumption, complex equipment, single pertinence and the like in the prior art for treating low-valent ions and COD in a water body, the invention provides the electro-adsorption material for removing the low-valent ions and COD in the water body and the preparation method thereof, which can realize the material utilization of the traditional mineral resources and also realize the purification of water pollutants.
In order to achieve the purpose, the invention adopts the following technical scheme:
an electro-adsorption material for removing water body low-valence ions and COD comprises the following components in parts by mass: low-grade (the grade of molybdenum is less than 3wt% and more than 0) molybdenum-containing sulphide ore 60-80 parts, molybdenite (the molybdenum content is more than 55 wt%) 10-20 parts, molybdenite tailings (the molybdenum content is less than 0.01wt% and more than 0) 10-20 parts are used as precursors 1, the precursors 1 are uniformly mixed, and then the superfine nano-particle MoO is formed through low-temperature oxidizing roasting and high-temperature volatilization3(ii) a The composition comprises the following components in parts by mass: 15-30 parts of graphite and brown30-50 parts of coal and 20-55 parts of weathered coal are used as a precursor 2, and the precursor 2 is uniformly mixed, roasted and subjected to superfine grinding to prepare an active substance carrier; ultrafine nano-particle MoO by adopting vapor deposition method3Uniformly loading the active substance carrier with the active substance carrier to obtain a composite material containing the active substance and the conductive substance; and then adding a binder, and molding to obtain the electro-adsorption material.
Further, the particle size of the precursor 1 is not more than 200 mu m, the carbon mass content in the precursor 2 is not less than 60%, and the particle size is not more than 200 mu m.
Further, the low-temperature oxidizing roasting temperature of the precursor 1 is 450-700 ℃, and the roasting time is 60 min.
Further, the high-temperature volatilization condition of the precursor 1 is under an air atmosphere, the temperature is 850-1050 ℃, and the treatment time is 30 min.
Further, the ultrafine nano-particle MoO3The particle size of the particles is 10 nm-100 nm.
Further, roasting the precursor 2 for 40-60 min at 1100-1300 ℃ in a nitrogen atmosphere; carrying out superfine grinding on the roasted product for 10-30 min by adopting a planetary ball mill to obtain an active substance carrier; the particle size of the active substance carrier particles is not more than 200 mu m.
Further, the mass content of molybdenum in the composite material is not less than 10%, and the average mass content of carbon is not less than 7%.
Further, the adhesive comprises the following components in parts by mass: 60-80 parts of humic acid, 10-25 parts of CMC, 10-15 parts of PVDF, and the amount of the binder is 5-10% of the mass of the composite material.
Further, the composite material was mixed with a binder and pressed into a cylindrical shape (diameter 0.1cm, height 10 cm) or a flat plate shape (length 10cm, width 10cm, thickness 0.1 cm).
The electro-adsorption material for removing the low-valence ions and COD in the water body is applied to removing the low-valence ions and COD in the wastewater, wherein the low-valence ions in the wastewater are K+、Na+、F-、Cl-One or more of the above (B), the total concentration is 40-500 mg/L; the COD content is 40-10000 mg/L; the pH value of the wastewater is 3-7. Further, K in the wastewater+、Na+、F-、Cl-The concentration of the (B) is 10-125 mg/L.
The invention has the following beneficial effects or advantages:
(1) the method realizes the resource utilization of low-grade minerals and slag;
(2) the method realizes the high-efficiency removal of low-valent ions in the water body and realizes the purification of the water body;
(3) the method has simple process and low cost, and is easy to realize industrialized application.
Drawings
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
The present invention will be further described with reference to the following specific examples. It should be noted that these examples are only for better understanding of the present invention, and do not limit the scope of the present invention.
In the following examples, the low-grade molybdenum-containing sulfide ore refers to molybdenum-containing sulfide ore with the molybdenum grade lower than 3wt%, the molybdenite refers to molybdenite with the molybdenum content higher than 55wt%, and the molybdenite tailings refer to molybdenite tailings with the molybdenum content lower than 0.01 wt%.
[ example 1 ]
Application of electro-adsorption material for removing low-valent ions and COD in water body in removing low-valent ions and COD in wastewater, namely K in water body+、Na+、F-、Cl-The total concentration is 40mg/L, the COD content is 500mg/L, the volume of the solution is 1000mL, and the pH value is 4.0.
As shown in fig. 1, the specific steps for preparing the electro-adsorption material are as follows: taking 80 parts of low-grade molybdenum-containing sulphide ore, 10 parts of molybdenite and 10 parts of molybdenite tailings as a precursor 1, wherein the particle size is 180 mu m; oxidizing and roasting the precursor 1 at 500 ℃ for 60min, and volatilizing the roasted product at 850 ℃ for 60min to form ultrafine nano-particle MoO3The particle size is 40 nm; the precursor 2 comprises 15 parts of graphite, 30 parts of lignite and 55 parts of weathered coal in parts by mass, wherein the carbon content is 63%, and the particle size is 170 mu m; the precursor 2 is 1100 under nitrogen atmosphereoC, roasting for 40 min; carrying out superfine grinding on the roasted product for 10min by adopting a planetary ball mill to obtain an active substance carrier, wherein the particle size is 100 mu m; ultrafine nano particle MoO volatilized at high temperature3The composite material is prepared by loading the molybdenum on an active substance carrier through vapor deposition, wherein the mass content of the molybdenum is 15%, and the average mass content of the carbon is 8%. The binder for preparing the electric adsorption material comprises, by mass, 60 parts of humic acid, 25 parts of CMC and 15 parts of PVDF, wherein the amount of the binder is 5% of the mass of the composite material; the composite material was mixed with a binder and pressed into a flat plate having a length of 10cm, a width of 10cm and a thickness of 0.1 cm. The electro-adsorption material is used for adsorbing and purifying water containing low-valence ions and high COD (chemical oxygen demand), the reaction time is 20min, the removal rate of the low-valence ions is 95.5%, the removal rate of the COD is 98.3%, and specific results are detailed in Table 1.
Table 1 example 1 specific parameters and results table
[ example 2 ]
Application of electro-adsorption material for removing low-valent ions and COD in water body in removing low-valent ions and COD in wastewater, namely K in water body+、Na+、F-、Cl-The total concentration is 100mg/L, the COD content is 1000mg/L, the volume of the solution is 1000ml, and the pH value is 5.0.
As shown in fig. 1, the specific steps for preparing the electro-adsorption material are as follows: taking 75 parts of low-grade molybdenum-containing sulfide ore, 12 parts of molybdenite and 13 parts of molybdenite tailings as a precursor 1, wherein the particle size is 170 mu m; oxidizing and roasting the precursor 1 at 550 ℃ for 70min, and volatilizing the roasted product at 900 ℃ for 80min to form ultrafine nano-particle MoO3The particle size is 50 nm; taking 18 parts of graphite, 32 parts of lignite and 50 parts of weathered coal in parts by mass as a precursor 2, wherein the carbon content is 55%, and the particle size is 170 mu m; the precursor 2 is placed under a nitrogen atmosphere 1150oC, roasting for 50 min; feeding the roasted product into a planetary ball millCarrying out superfine grinding for 15min to obtain an active substance carrier, wherein the particle size is 80 mu m; ultrafine nano particle MoO volatilized at high temperature3The composite material is prepared by loading the molybdenum on an active substance carrier through vapor deposition, wherein the mass content of the molybdenum is 10%, and the average mass content of the carbon is 10%. The binder for preparing the electric adsorption material comprises 65 parts of humic acid, 22 parts of CMC and 13 parts of PVDF by mass, and the using amount of the binder is 6.5 percent of the mass of the composite material; the composite material was mixed with a binder and pressed into a flat plate having a length of 10cm, a width of 10cm and a thickness of 0.1 cm. The electro-adsorption material is used for adsorbing and purifying water containing low-valence ions and high COD (chemical oxygen demand), the reaction time is 20min, the removal rate of the low-valence ions reaches 95.8%, the removal rate of the COD is 98.7%, and specific results are detailed in Table 2.
Table 2 example 2 specific parameters and results table
[ example 3 ]
Application of electro-adsorption material for removing low-valent ions and COD in water body in removing low-valent ions and COD in wastewater, namely K in water body+、Na+、F-、Cl-The total concentration is 300mg/L, the COD content is 2000mg/L, the volume of the solution is 1000ml, and the pH value is 6.0.
As shown in fig. 1, the specific steps for preparing the electro-adsorption material are as follows: taking 70 parts of low-grade molybdenum-containing sulphide ore, 18 parts of molybdenite and 12 parts of molybdenite tailings as a precursor 1, wherein the particle size is 175 mu m; oxidizing and roasting the precursor 1 at the temperature of 600 ℃ for 80min, and volatilizing the roasted product at the temperature of 1000 ℃ for 75min to form ultrafine nano-particle MoO3The particle size is 30 nm; taking 20 parts of graphite, 40 parts of lignite and 40 parts of weathered coal in parts by mass as a precursor 2, wherein the carbon content is 68%, and the particle size is 150 mu m; the precursor 2 is put under the nitrogen atmosphere 1200oC, roasting for 60 min; carrying out superfine grinding on the roasted product for 15min by adopting a planetary ball mill to obtain an active substance carrier, wherein the particle size is 70 mu m; ultrafine nano particle MoO volatilized at high temperature3The composite material is prepared by loading the molybdenum on an active substance carrier through vapor deposition, wherein the mass content of the molybdenum is 12%, and the average mass content of the carbon is 12%. The binder for preparing the electric adsorption material comprises 70 parts of humic acid, 15 parts of CMC and 15 parts of PVDF by mass, and the using amount of the binder is 8 percent of the mass of the composite material; the composite material was mixed with a binder and pressed into a flat plate having a length of 10cm, a width of 10cm and a thickness of 0.1 cm. The electro-adsorption material is used for adsorbing and purifying water containing low-valence ions and high COD (chemical oxygen demand), the reaction time is 20min, the removal rate of the low-valence ions reaches 96.1%, the removal rate of the COD is 98.2%, and specific results are detailed in Table 3.
Table 3 example 3 specific parameters and results table
Claims (6)
1. An electro-adsorption material for removing water body low-valent ions and COD is characterized by comprising the following components in parts by mass: 60-80 parts of low-grade molybdenum-containing sulfide ore, 10-20 parts of molybdenite and 10-20 parts of molybdenite tailings as precursors 1, uniformly mixing the precursors 1, and performing low-temperature oxidizing roasting and high-temperature volatilization to form ultrafine nano-particle MoO3(ii) a The composition comprises the following components in parts by mass: taking 15-30 parts of graphite, 30-50 parts of lignite and 20-55 parts of weathered coal as a precursor 2, uniformly mixing the precursor 2, roasting and carrying out superfine grinding to obtain an active substance carrier; using vapor deposition to form ultrafine nano-particle MoO3Uniformly loading the active substance carrier with the active substance carrier to obtain a composite material containing the active substance and the conductive substance; then adding a binder, and forming to prepare the electro-adsorption material; the low-temperature oxidizing roasting temperature of the precursor 1 is 450-700 ℃, and the roasting time is 60 min; the high-temperature volatilization condition of the precursor 1 is that the temperature is 850-1050 ℃ under the air atmosphere, and the treatment time is 30 min; the ultrafine nano-particle MoO3The particle size of the (B) is 10 nm-100 nm; the adhesive comprises the following components in parts by mass: 60-80 parts of humic acid, 10-25 parts of CMC, 10-15 parts of PVDF, and the amount of the binder is 5-10% of the mass of the composite material.
2. The electro-adsorption material for removing low-valent ions and COD in the water body according to claim 1, characterized in that the particle size of the precursor 1 is not higher than 200 μm, the carbon mass content in the precursor 2 is not lower than 60%, and the particle size is not higher than 200 μm.
3. The electro-adsorption material for removing water body low-valent ions and COD according to claim 1, characterized in that the precursor 2 is roasted at 1100-1300 ℃ for 40-60 min in a nitrogen atmosphere; carrying out superfine grinding on the roasted product for 10-30 min by adopting a planetary ball mill to obtain an active substance carrier; the particle size of the active substance carrier particles is not higher than 200 mu m.
4. The electro-adsorption material for removing low-valent ions and COD in a water body according to claim 1, wherein the composite material has a molybdenum mass content of not less than 10% and a carbon average mass content of not less than 7%.
5. The electro-adsorption material for removing low-valent ions and COD in a water body according to claim 1, wherein the composite material is mixed with a binder and pressed into a cylindrical shape or a flat plate shape.
6. The application of the electro-adsorption material for removing low-valent ions and COD in water body according to claim 1, wherein the low-valent ions in the wastewater are K+、Na+、F-、Cl-The total concentration of the four ingredients is 50-500 mg/L; the COD content is 50-10000 mg/L; the pH value of the wastewater is 3-7.
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