CN114054472A - Method for degrading halogen-containing organic pollutants - Google Patents
Method for degrading halogen-containing organic pollutants Download PDFInfo
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- CN114054472A CN114054472A CN202111237725.9A CN202111237725A CN114054472A CN 114054472 A CN114054472 A CN 114054472A CN 202111237725 A CN202111237725 A CN 202111237725A CN 114054472 A CN114054472 A CN 114054472A
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- halogen
- containing organic
- ball milling
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- persulfate
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09B—DISPOSAL OF SOLID WASTE
- B09B3/00—Destroying solid waste or transforming solid waste into something useful or harmless
Abstract
The invention discloses a method for degrading halogen-containing organic pollutants, which is characterized by comprising the following steps: halogen-containing organic matters, persulfate and calcium oxide are mixed and then degraded by adopting a mechanical ball milling method. The invention provides a method for degrading halogen-containing organic pollutants efficiently and thoroughly, which takes persulfate as an abrasive and calcium oxide as a grinding aid, and activates persulfate through electron transfer, alkali activation, energy transfer and other ways during the mechanical ball milling process to release hydroxyl radicals and sulfate radicals from the persulfate. And the mechanical ball milling has the characteristics of mild reaction conditions, simple operation, wide application range, no secondary pollution and the like, and particularly has obvious advantages in dehalogenation and mineralization of halogen-containing organic pollutants.
Description
Technical Field
The invention relates to the technical field of degradation of halogen-containing organic pollutants, in particular to a method for degrading halogen-containing organic pollutants.
Background
Currently, methods commonly used to treat halogen-containing organic contaminants include incineration, biological, catalytic, mechanical ball milling, and the like. Among them, the high-temperature incineration method has too high energy consumption cost, and other toxic and harmful substances can be generated in the disposal process to cause secondary pollution; the treatment time of the biodegradation technology is long, and the degradation effect is not high enough; the catalytic method also has problems of severe treatment conditions and difficulty in scale-up. The mechanical ball milling method for treating the halogen-containing organic pollutants has the characteristics of mild reaction conditions, simple operation, wide application range, no secondary pollution and the like, and particularly has obvious advantages in dehalogenation and mineralization of the halogen-containing organic pollutants. However, at present, the degradation of halogen-containing organic matters by adopting a mechanical ball milling method is not reported, and the main reasons are as follows: halogen-containing organic substances have lipophilicity and hydrophobicity, so that the halogen-containing organic substances easily enter food chains and are accumulated in fat tissues, and pose a threat to human health.
Therefore, further improvements are needed in the existing processes for halogen-containing organic contaminants.
Disclosure of Invention
The invention aims to solve the technical problem of providing a method for degrading halogen-containing organic pollutants, which has high degradation rate of halogen-containing organic pollutants and does not have secondary pollution.
The technical scheme adopted by the invention for solving the technical problems is as follows: a method of degrading halogen-containing organic contaminants, characterized by: halogen-containing organic matters, persulfate and calcium oxide are mixed and then degraded by adopting a mechanical ball milling method.
Preferably, the halogen-containing organic matter is pretreated before ball milling, the halogen-containing organic matter is dried at 45-55 ℃, then is smashed, is added with a molecular sieve with the diameter of 1.2-2.0mm and cabot carbon black for grinding, passes through a 80-mesh screen, and finally is subjected to magnetic separation to remove magnetic substances in the magnetic separation. The molecular sieve and the organic halide are premixed firstly, which is beneficial to the ball milling and mixing in the next step. The molecular sieve has no direct removing effect on the organic halide, but in the subsequent ball milling process, a limited domain effect can be generated under the action of the molecular sieve, after the limited domain, the halogen-containing organic matter and the persulfate carry out local high-concentration reaction in a tiny space, so that the reaction efficiency is improved, the cabot carbon black also has no direct removing effect, but in the subsequent ball milling process, free electrons generated by calcium oxide can be more quickly guided to the surface of the persulfate under the action of the cabot carbon black to generate sulfate radicals and hydroxyl radicals, so that the reaction efficiency is improved.
Preferably, the mass ratio of the halogen-containing organic substance to the molecular sieve to the cabot black is 15:1:1 to 25:1: 1.
Preferably, the mass ratio of the total mass of the halogen-containing organic substance, the persulfate and the calcium oxide to the grinding ball is 1: 20-50; the mass ratio of the halogen-containing organic matter to the persulfate to the calcium oxide is 1:1: 1-1: 10: 10. The mass ratio of the material balls is too low, so that the ball milling tank is filled with the grinding balls, and the grinding balls do not have enough space to fully move, so that the impact of the grinding balls is also reduced, and the degradation effect on organic pollutants is weakened; the mass ratio of the material balls is too high, so that the effective impact of the grinding balls on the material is less, the accumulation of energy in the system is also lower, and the degradation effect is also reduced. In the mass ratio of the halogen-containing organic matter, the persulfate and the calcium oxide, if the content of the halogen-containing organic matter is too high and the mass sum of the persulfate and the calcium oxide is too low, the persulfate cannot be in full contact with the calcium oxide and cannot be well activated, so that the removal efficiency is reduced; if the content of the halogen-containing organic substance is too low and the sum of the mass of the persulfate and the mass of the calcium oxide is too high, the persulfate may directly and sufficiently contact with the halogen-containing organic substance and cannot be well activated, so that the removal efficiency is reduced. Under the appropriate mass ratio, the calcium oxide grinding aid can release free electrons in the ball milling process, so that the persulfate grinding agent is effectively activated, sulfate radicals and hydroxyl radicals with strong oxidizing property can be generated under the ball milling condition after the persulfate grinding agent is activated by the free electrons, the radicals attack halogen-containing organic matters, the carbon halogen bonds of the halogen-containing organic matters are destroyed, the ring opening reaction is carried out, meanwhile, the persulfate can oxidize the halogen-containing organic matters, and the purpose of degrading the halogen-containing organic matters is achieved.
Preferably, the rotation speed of the ball mill is 800-1500 rpm, and the grinding time is 3-5 h. The energy generated by too low ball mill rotation speed and too little grinding time can not enable calcium oxide to fully activate persulfate, so that the degradation effect can not be achieved, and the generation of secondary pollutants can be possibly caused by too high ball mill rotation speed and too long grinding time, so that the degradation purpose can not be achieved.
Preferably, the ball milling mode of the ball mill is vibration ball milling, the material of the grinding balls and the ball milling tank is 316 stainless steel, the size of the balls is 8-10mm, the volume of the ball milling tank is 200mL, and the total mass of the halogen-containing organic matter, the sodium persulfate and the calcium oxide added each time is 10-20 g. The vibration ball milling is carried out in a vibration and swing mode, compared with the traditional ball mill, the vibration ball milling device is easy to carry out amplification experiments, has lower energy consumption and can contain more pollutants, thereby being capable of degrading more halogen-containing organic matters at one time. The grinding ball made of stainless steel has high collision energy and is economical and durable. If the size is too small, the generated collision energy is low due to light weight, and the grinding agent cannot be effectively activated if the input energy is not reached, so that pollutants cannot be completely degraded. The large-size grinding balls can generate larger collision energy, but because the large-size grinding balls are limited by the volume of the ball milling tank, the number of the grinding balls which can be placed is small, so that the impact frequency is low, the generated energy is insufficient, the capacity of degrading pollutants is reduced, dead angles are easily generated when the large-size grinding balls move in the ball milling tank, the full ball milling of materials is not facilitated, the ball milling reaction is insufficient, and the pollutants cannot be completely degraded.
Preferably, the persulfate is sodium persulfate.
Preferably, the halogen-containing organic substance is at least one of 2, 4-dichlorophenol, hexachloroethane, 1,2,4, 5-tetrachlorobenzene, pentachloronitrobenzene and tetrabromobisphenol A.
Preferably, the degradation rate of the halogen-containing organic substance is 90% or more.
Compared with the prior art, the invention has the advantages that: the invention provides a method for degrading halogen-containing organic pollutants efficiently and thoroughly, which takes persulfate as an abrasive and calcium oxide as a grinding aid, and activates persulfate through electron transfer, alkali activation, energy transfer and other ways during the mechanical ball milling process to release hydroxyl radicals and sulfate radicals from the persulfate. And the mechanical ball milling has the characteristics of mild reaction conditions, simple operation, wide application range, no secondary pollution and the like, and particularly has obvious advantages in dehalogenation and mineralization of halogen-containing organic pollutants.
Detailed Description
The present invention will be described in further detail with reference to examples.
The invention provides 4 examples and 2 comparative examples, wherein halogen-containing organic matters are pretreated before ball milling, the halogen-containing organic matters are dried in a vacuum drying oven at 50 ℃, then are mashed, 0.05g of SBA-15 molecular sieve with the diameter of 1.2-2.0mm and 0.05g of REGAL 400R cabot carbon black are added for grinding, the mixture passes through an 80-mesh screen, and finally a magnetic separator is adopted for removing magnetic substances in the mixture.
Example 1
Weighing 1g of 2, 4-dichlorophenol, 6.5g of calcium oxide and 6.5g of sodium persulfate, placing 420g of 316 stainless steel balls with different diameters of 8-10mm in a 200mL 316 stainless steel ball milling tank, placing the ball milling tank in a ball mill, wherein the ball milling mode is vibration ball milling, the set rotating speed is 1200rpm, the time is 3h, the ball milling process is working for 30min, the interval is 5min, and the processes are sequentially and circularly carried out. The samples before and after the reaction were subjected to processes of dissolution, sonication, centrifugation, filtration, dilution, etc., and measured using a gas chromatograph.
Example 2
Weighing 1g of hexachloroethane, 6.5g of calcium oxide and 6.5g of sodium persulfate, placing 420g of 316 stainless steel balls with different diameters of 8-10mm in a 200mL 316 stainless steel ball milling tank, placing the ball milling tank in a ball mill, wherein the ball milling mode is vibration ball milling, the set rotating speed is 1000rpm, the time is 5 hours, the ball milling process is 30min, the interval is 5min, and the processes are sequentially and circularly carried out. The samples before and after the reaction were subjected to processes of dissolution, sonication, centrifugation, filtration, dilution, etc., and measured using a gas chromatograph.
Example 3
Weighing 1g of 1,2,4, 5-tetrachlorobenzene, 6.5g of calcium oxide and 6.5g of sodium persulfate, putting 420g of 316 stainless steel balls with different diameters of 8-10mm into a 200mL 316 stainless steel ball milling tank, putting the ball milling tank into a ball mill, wherein the ball milling mode is vibration ball milling, the set rotating speed is 800rpm, the time is 5 hours, the ball milling process is 30min of work, the interval is 5min, and the processes are sequentially and circularly carried out. The samples before and after the reaction were subjected to processes of dissolution, sonication, centrifugation, filtration, dilution, etc., and measured using a gas chromatograph.
Example 4
Weighing 1g of tetrabromobisphenol A, 6.5g of calcium oxide and 6.5g of sodium persulfate, placing 420g of 316 stainless steel balls with different diameters of 8-10mm in a 200mL 316 stainless steel ball milling tank, placing the ball milling tank in a ball mill, wherein the ball milling mode is vibration ball milling, the set rotating speed is 1200rpm, the time is 3h, the ball milling process is work for 30min, the interval is 5min, and the processes are sequentially and circularly carried out. The samples before and after the reaction were subjected to processes of dissolution, sonication, centrifugation, filtration, dilution, etc., and measured using liquid chromatography.
Comparative example 1
Weighing 1g of tetrabromobisphenol A, 420g of 316 stainless steel balls with different diameters of 8-10mm and 200mL of ball milling tank, placing the ball milling tank in a ball mill, wherein the ball milling mode is vibration ball milling, the set rotating speed is 1200rpm, the time is 5h, the ball milling process is working for 30min, the interval is 5min, and the working is carried out in a circulating mode in turn. The samples before and after the reaction were subjected to processes of dissolution, sonication, centrifugation, filtration, dilution, etc., and measured using liquid chromatography.
Comparative example 2
Weighing tetrabromobisphenol A1 g, Fe-SO26.5g of reagent, 420g of 316 stainless steel balls with different diameters of 8-10mm and 200mL of ball milling tank, wherein the ball milling tank is arranged in a ball mill, the ball milling mode is vibration ball milling, the set rotating speed is 1200rpm, the time is 5h, the ball milling process is working for 30min, the interval is 5min, and the processes are carried out in a circulating mode in turn. The samples before and after the reaction were subjected to processes of dissolution, sonication, centrifugation, filtration, dilution, etc., and measured using liquid chromatography.
The obtained 4 examples and 2 comparative examples were tested before and after ball milling of contaminants by the following specific test methods:
before and after ball milling, 0.05g of each material in the tank is taken out and put into a 10mL centrifuge tube, 10mL of normal hexane is added, ultrasonic dissolution is carried out for 20min, centrifugation is carried out at 8000rpm for 1min, the material is filtered by a 0.25 mu m organic filter membrane and then is to be detected, the type of a high performance gas chromatography used in the experiment is Agilent 6890, a chromatographic column is an HP-INNOWAX capillary column (30m multiplied by 0.32mm multiplied by 0.5 mu m), and a flame ionization detector is adopted. After 4 hours of treatment, the contaminated concentration of 2, 4-dichlorophenol before ball milling in example 1 was 71.4mg/kg, and the contaminated concentration of 2, 4-dichlorophenol after ball milling was 0 mg/kg. Example 2 the contaminated concentration of hexachloroethane before ball milling was 71.4mg/kg, and the contaminated concentration of hexachloroethane after ball milling was 0.65 mg/kg. Example 3 the contaminated concentration of 1,2,4, 5-tetrachlorobenzene before ball milling was 71.4mg/kg, and the contaminated concentration of 1,2,4, 5-tetrachlorobenzene after ball milling was 0.65 mg/kg. Example 4 the concentration of tetrabromobisphenol A contaminant before ball milling was 71.4mg/kg, and the concentration of tetrabromobisphenol A contaminant after ball milling was 0 mg/kg. Comparative example 1 the concentration of tetrabromobisphenol a contamination before ball milling was 71.4mg/kg, and the concentration of tetrabromobisphenol a contamination after ball milling was 71.4 mg/kg. Comparative example 2 the concentration of tetrabromobisphenol a contamination before ball milling was 71.4mg/kg, and the concentration of tetrabromobisphenol a contamination after ball milling was 44.3 mg/kg.
Under the conditions of proper mass ratio, rotation speed, grinding ball size and material, the calcium oxide grinding aid can release free electrons in the ball milling process, the free electrons are quickly transferred to the surface of the persulfate grinding agent under the action of the carbon black, the persulfate grinding agent can be activated after the free electrons are captured, the activated persulfate grinding agent can generate sulfate radicals and hydroxyl radicals with strong oxidizing property under the ball milling condition, the radicals attack halogen-containing organic matters, generating a confinement effect under the influence of the molecular sieve, after the confinement, the halogen-containing organic matter and the persulfate perform local high-concentration reaction in a tiny space to destroy the carbon-halogen bond and generate ring-opening reaction, meanwhile, inorganic substances such as sodium sulfate, sodium chloride and the like are generated to achieve the purpose of harmlessness of pollutants, and in addition, the halogen-containing organic substances can be oxidized after energy in the ball milling process is transferred to persulfate, so that the purpose of degrading the halogen-containing organic pollutants is achieved.
Claims (9)
1. A method of degrading halogen-containing organic contaminants, characterized by: halogen-containing organic matters, persulfate and calcium oxide are mixed and then degraded by adopting a mechanical ball milling method.
2. A method for degrading halogen-containing organic pollutants according to claim 1, characterized in that: the method comprises the steps of pretreating the halogen-containing organic matters before ball milling, drying the halogen-containing organic matters at 45-55 ℃, mashing, adding a molecular sieve with the diameter of 1.2-2.0mm and cabot carbon black, grinding, sieving with a 80-mesh sieve, and finally removing magnetic substances in the mixture by using a magnetic separator.
3. A method for degrading halogen-containing organic pollutants according to claim 2, characterized in that: the mass ratio of the halogen-containing organic matter to the molecular sieve to the cabot carbon black is 15:1: 1-25: 1: 1.
4. A method for degrading halogen-containing organic pollutants according to claim 1, characterized in that: the mass ratio of the total mass of the halogen-containing organic matters, the persulfate and the calcium oxide to the mass of the grinding balls is 1: 20-50; the mass ratio of the halogen-containing organic matter to the persulfate to the calcium oxide is 1:1: 1-1: 10: 10.
5. A method for degrading halogen-containing organic pollutants according to claim 1, characterized in that: the rotation speed of the ball mill is 800-1500 rpm, and the grinding time is 3-5 h.
6. A method for degrading halogen-containing organic pollutants according to claim 1, characterized in that: the ball milling mode of the ball mill is that the materials of vibration ball milling balls and a ball milling tank are 316 stainless steel, the size of the balls is 8-10mm, the volume of the ball milling tank is 200mL, and the total mass of the added halogen-containing organic matter, sodium persulfate and calcium oxide is 10-20 g each time.
7. A method for degrading halogen-containing organic pollutants according to claim 1, characterized in that: the persulfate is sodium persulfate.
8. A method for degrading halogen-containing organic pollutants according to claim 1, characterized in that: the halogen-containing organic pollutant is at least one of 2, 4-dichlorophenol, hexachloroethane, 1,2,4, 5-tetrachlorobenzene, pentachloronitrobenzene and tetrabromobisphenol A.
9. A method for degrading halogen-containing organic contaminants according to any of claims 1 to 8, characterized in that: the degradation rate of the halogen-containing organic matters is more than 90%.
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