CN114477412A - Method for removing organic pollutants in water by thermally activating persulfate - Google Patents
Method for removing organic pollutants in water by thermally activating persulfate Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/722—Oxidation by peroxides
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/02—Treatment of water, waste water, or sewage by heating
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2303/00—Specific treatment goals
- C02F2303/10—Energy recovery
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/02—Specific form of oxidant
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/02—Specific form of oxidant
- C02F2305/023—Reactive oxygen species, singlet oxygen, OH radical
Abstract
The invention belongs to the technical field of water treatment, and discloses a method for removing organic pollutants in water by thermally activating persulfate, which takes wastewater containing organic pollutants to be treated as reaction liquid, controls the temperature to be above 40 ℃, and adds persulfate into the reaction liquid for reaction; in the reaction process, persulfate can be activated in a thermal environment to generate free radicals, attack organic pollutants to generate organic free radicals, and then perform polymerization reaction to generate organic solid particle precipitates; and (4) carrying out solid-liquid separation after the reaction, wherein the liquid obtained by separation is the treated wastewater. According to the invention, complete degradation of organic matters is not pursued, but most of organic pollutants are subjected to polymerization reaction to form solid organic particles, and most of organic pollutants can be removed from water through solid-liquid separation after the reaction is finished, so that the technical problems of high persulfate consumption and low total organic matter removal efficiency in the prior art are solved.
Description
Technical Field
The invention belongs to the technical field of water treatment, and particularly relates to a method for removing organic pollutants in water by thermally activating persulfate.
Background
Industries such as textile, paper, brewing, slaughtering and petrochemical industries emit a large amount of organic waste water during production activities. The wastewater has the characteristics of high organic content and difficult degradation, and the temperature of some wastewater is higher, which is traditionalThe biochemical treatment modes such as A/A/O, UASB, biological aerated filter and the like or the physicochemical treatment modes such as adsorption, coagulation and the like are difficult to realize the high-efficiency removal of organic pollutants, and the mineralization rate of the organic matters is generally below 50 percent or even lower. Advanced oxidation technology is generally applied to the pretreatment or advanced treatment of such wastewater and shows great advantages, and the reaction can be divided into two processes: (1) the oxidant is activated or catalyzed by light, electricity, heat, catalyst and the like to generate SO with strong oxidizing property4 ·-And HO·Isoradicals; (2) the free radicals attack organic pollutants by means of addition, hydrogen abstraction, electron transfer and the like on unsaturated bonds, so that the organic pollutants are decomposed into small molecular organic matters such as formic acid, acetic acid and the like or are completely mineralized into CO2. The advanced oxidation technology is a main method which can effectively degrade toxic, harmful and nonbiodegradable organic pollutants at present.
In recent years, the persulfate-based advanced oxidation technology has been widely studied and applied due to its advantages of wide pH application range, long radical lifetime, and little influence from background substances. The persulfate may be activated by heat, ultraviolet light, transition metals, bases, and phenol quinones. Thermally activating persulfate means that high activity SO is generated by activating persulfate at high temperature4 ·-Or HO·Free radicals attack organic pollutants by means of addition, hydrogen abstraction, electron transfer and the like, so that the pollutants are decomposed into small molecular substances and even completely mineralized. Because the process is efficient and rapid, and the mineralization rate of organic matters is high, the method is widely applied to the aspects of underground water treatment, soil remediation and the like.
However, the thermally activated persulfate technology has some defects in the water treatment process (for example, a method for removing COD from high-salt coal chemical wastewater by thermally activated persulfate disclosed in CN108996656A and a method for treating high-temperature printing and dyeing wastewater disclosed in CN 101525178A): (1) the reaction time is long, the solution temperature needs to be maintained for a long time until most target pollutants are oxidized and decomposed into micromolecular organic matters and even completely mineralized, and the energy consumption is large; (2) the path for degrading target pollutants into small molecular substances is long, the consumption of the oxidant (persulfate) is high, and the utilization rate is low; (3) the treated organic wastewater still contains a large amount of organic substances, and the removal rate of COD or TOC is not high: (4) other derivative organic matters with higher toxicity can be generated in the process of oxidative degradation of the organic pollutants, so that the subsequent treatment is not facilitated.
Disclosure of Invention
In view of the above drawbacks or needs for improvement of the prior art, the present invention provides a method for removing organic pollutants from water by thermally activating persulfate, which adjusts the addition amount of persulfate as an oxidant according to the amount of the pollutants and controls the reaction time, and allows the organic matters to form macromolecular polymers without pursuing complete degradation of the organic matters. In this process, SO is generated from the oxidizing agent4 ·-And HO·The free radicals mainly play a role in initiating a polymerization chain reaction, along with the occurrence of a chain growth reaction, the molecular weight of an organic polymer is increased, the hydrophobicity is enhanced, and finally the organic polymer is separated out from water to form solid particles, and then most organic pollutants can be removed from the water through solid-liquid separation, so that the technical problems of high persulfate consumption and low total organic matter removal efficiency in the prior art are solved, and the effect of recovering a carbon source is achieved. The invention can solve the problems of slow degradation rate of organic pollutants in water and low removal rate of COD and TOC, and has the advantages of wide pH adaptation range, capability of recovering organic resources, reduction of generation of toxic derivatives and reduction of difficulty of subsequent biological treatment process.
In order to achieve the above object, according to the present invention, there is provided a method for removing organic contaminants from water by thermally activating persulfate, which is characterized in that waste water containing organic contaminants to be treated is used as a reaction liquid, the reaction liquid is controlled to have a temperature of 40 ℃ or higher, and persulfate is added to the reaction liquid to carry out a reaction; the ratio of the amount of the persulfate to the amount of the organic pollutant in the reaction solution is 0.5-50: 1; in the reaction process, the persulfate can be activated in a thermal environment to generate free radicals, attack organic pollutants to generate organic free radicals, and then perform polymerization reaction to generate organic solid particle precipitates; and (3) carrying out solid-liquid separation on the reaction system after reacting for 3-210 minutes, wherein the liquid obtained by separation is the treated wastewater.
As a further preferred of the present invention, the persulfate includes at least one of Peroxymonosulfate (PMS), Peroxydisulfate (PDS); the ratio of the amount of the persulfate to the volume of the reaction solution is preferably 0.5 to 1000 mmol/L.
As a further preference of the present invention, when the persulfate comprises Peroxymonosulfate (PMS), the chemical reactions that specifically occur during the reaction include, but are not limited to:
SO4 ·-+ organic contaminant → SO4 2-+ organic solid polymer particles + soluble oxidation products,
HO·+ organic contaminants → HO-+ organic solid polymer particles + soluble oxidation products;
when the persulfate salt comprises a peroxydisulfate salt (PDS), specific chemical reactions that occur during the reaction include, but are not limited to:
SO4 ·-+ organic contaminants → SO4 2-+ organic solid polymer particles + soluble oxidation products,
HO·+ organic contaminants → HO-+ organic solid polymer particles + soluble oxidation products.
In a further preferred embodiment of the present invention, the temperature of the reaction solution is specifically controlled to 40 to 99 ℃.
Further preferably, the temperature of the reaction solution is controlled to 40 ℃ or higher by heating, or by directly using high-temperature waste water satisfying the temperature requirement, or by mixing 2 types of waste water having higher or lower temperatures;
the attack organic contaminant is to attack the organic contaminant by means of addition or hydrogen abstraction or electron transfer.
As a further preference of the present invention, the reaction is preferably carried out under stirring conditions; more preferably, the stirring conditions are achieved by mechanical stirring or aeration stirring.
In a further preferred embodiment of the present invention, the organic contaminant in the wastewater containing organic contaminants to be treated is one or more of a phenolic organic substance, an aniline organic substance, an alkoxybenzene organic substance, a nitrobenzene organic substance, a phenolic ester organic substance, a benzene or biphenyl organic substance, and a heterocyclic compound.
As a further preference of the present invention, the solid-liquid separation is achieved by means of coagulating sedimentation or filtration or centrifugal separation or static sedimentation.
Compared with the existing method for removing organic pollutants in water by thermally activating persulfate, the method for removing organic pollutants in water does not need to degrade the organic pollutants into micromolecules or even mineralize the organic pollutants to improve the removal rate of COD and TOC in the wastewater, but promotes the organic pollutants to have polymerization reaction by controlling the reaction time and the addition of the oxidant persulfate to generate organic solid polymer particles, and then removes the original organic pollutants by simple solid-liquid separation. When the method achieves the same total organic matter removal rate, the method has the advantages of less oxidant consumption, shorter reaction time and more heat energy saving, and organic carbon resources can be recovered and reused because the solid obtained by solid-liquid separation after the reaction is an organic polymer.
According to the method, the addition amount of the oxidant persulfate is controlled according to the amount of the organic pollutant substances in the reaction system, the reaction time is controlled to be 3-210 minutes, so that the organic matters are in a partially oxidized state, and the phenomenon that the organic matters are completely oxidized due to overlong reaction time or high-concentration oxidant can be avoided. The invention does not need high-concentration oxidant to provide a very large amount of active free radicals to mineralize and degrade organic matters, and only needs relatively less high-activity free radicals to carry out the chain initiation process. The invention converts most of the organic matters in the water into separable solid particles, and in addition, a small amount of soluble organic matters can be removed in a coprecipitation mode with the polymer, and little organic matters remain in the filtered water. In addition, the polymer produced by the method is a carbon-containing organic substance and can be recycled.
Compared with the prior art that the thermal activation persulfate degrades single wastewater, the method can treat various types of organic pollutant wastewater, and has wider application range. Compared with the prior art that the thermal activation persulfate degrades the organic wastewater, the method does not need to adjust the pH value of the reaction liquid, can achieve better effect under the acidic, neutral or alkaline conditions, reduces the use of medicaments, reduces secondary pollution and saves cost. In addition, compared with the existing thermal activation persulfate degradation high-temperature wastewater, the method provided by the invention can remove organic pollutants at the same temperature, and has the advantages of shorter reaction time and higher efficiency, wherein the COD and TOC removal rate is more than 80%.
In general, compared with the prior art, the above technical solution contemplated by the present invention can achieve the following beneficial effects:
(1) the organic pollutant removal reaction path is short, the reaction time is short, the total organic matter removal is quick and effective, and the removal rate of COD and TOC is high;
(2) the process is simple to operate, and no additional equipment is needed;
(3) the waste heat of the high-temperature waste water can be utilized, and energy is saved;
(4) the pH is not required to be adjusted, and the acid, neutral and alkaline effects can achieve better treatment effects;
(5) the possibility of generating toxic derivatives is reduced, and the difficulty of subsequent treatment is reduced;
(6) the consumption of the oxidant persulfate is low, the utilization rate is high, and resources are saved;
(7) organic carbon resources and energy can be recovered by separating the organic solid polymer produced after the reaction.
Drawings
FIG. 1 is a graph showing the removal of phenol with time obtained after filtration of the reaction liquid in example 1.
FIG. 2 is a graph showing the TOC removal obtained after filtration of the reaction solution in the heat/PDS/phenol system in example 1.
FIG. 3 is a graph showing the polymerization rate of phenol according to pH in example 4.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention. In addition, the technical features involved in the embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
The method for removing organic pollutants in water by thermally activating persulfate in the invention generally comprises the steps of forming a reaction system by wastewater containing organic pollutants and persulfate, controlling the temperature of the solution to be more than 40 ℃, controlling the concentration of the persulfate (the concentration of the persulfate can be controlled to be 0.5-1000 mmol/L), reacting for 3-210 minutes, polymerizing the organic pollutants to generate solid particle precipitates, dispersing the solid particle precipitates in reaction liquid, and carrying out solid-liquid separation on the reaction liquid after the reaction is finished, wherein the solid is a carbon-containing organic polymer, and the liquid is the treated wastewater.
Example 1
This example compares the removal of phenol and COD in a PDS/phenol system, a thermal/phenol system and a thermal/PDS/phenol system. The results, which show that phenol and COD were not substantially removed in the persulfate/phenol system and the heat/phenol system, whereas phenol was completely removed after 30 minutes and organic solid polymer particles were formed in the heat/PDS/phenol system, indicate that PDS alone or heating alone did not remove phenol from solution (as shown in figure 1, the data essentially coincided with the "persulfate alone" condition and the "heating alone" condition), but that phenol removal reactions occurred only when heating and PDS was present (as shown in figure 1).
The specific implementation parameters of the heat/PDS/phenol system are as follows:
the phenol concentration: 1mmol/L
The PDS concentration: 10mmol/L
Volume of reaction solution: 200mL
Temperature of the reaction solution: 80 deg.C
pH of the reaction solution: 3.5
The specific implementation parameters of the PDS/phenol system are as follows:
the phenol concentration: 1mmol/L
The PDS concentration: 10mmol/L
Volume of reaction solution: 200mL
Temperature of the reaction solution: 25 deg.C
pH of the reaction solution: 3.5
The specific implementation parameters of the heat/phenol system are as follows:
the phenol concentration: 1mmol/L
The PDS concentration: 0
Volume of reaction solution: 200mL
Temperature of the reaction solution: 80 deg.C
pH of the reaction solution: 3.5
Example 2
This example compares the removal of phenol and total organic TOC in a thermal/PDS/phenol system at five different temperatures, 50 deg.C, 60 deg.C, 70 deg.C, 80 deg.C, and 90 deg.C. The remaining parameters, except for temperature, were the same as for the heat/PDS/phenol system in example 1. The results show that as the solution temperature increases, the phenol and TOC removal rates increase. Wherein, at 80 ℃, phenol can be completely removed within 30 minutes, and TOC removal rate of more than 90 percent can be achieved within 35 minutes. Organic solid polymer particles are generated in the reaction process, and the generation amount of the solid particles shows a trend of increasing firstly and then decreasing with the increase of the temperature.
Example 3
This example compares the effect of five different concentrations of persulfate at 5, 10, 15, 20, 25mmol/L on phenol degradation and COD removal for a heat/PDS/phenol system. The same parameters as for the heat/PDS/phenol system of example 1 were used, except for the persulfate concentration. Along with the increase of the concentration of the persulfate, the removal of phenol and COD is also quickened, organic solid polymer particles are generated in the reaction process, and the proportion (polymerization rate) of the generated organic solid polymer particles in the total organic matters under different persulfate concentrations is more than 80%.
Example 4
This example compares the removal of phenol and COD at different pH's for the thermal/PDS/phenol system at pH's of 1, 5, 7, 9, 11. The parameters, except for the pH, were the same as for the heat/PDS/phenol system in example 1. As the pH increases, the removal of phenol and COD hardly affects, and organic solid polymer particles are generated in the reaction process, but the generation amount of solid particles is reduced along with the increase of alkalinity.
Example 5
The removal of o-, m-and p-cresol by the heat-activated persulfate system was investigated in this example. The experimental parameters were the same as for the heat/PDS/phenol system of example 1, except that the phenol in the heat/PDS/phenol system was replaced. The results show that o-cresol, m-cresol and p-cresol undergo polymerization in the system to generate tan, khaki and white organic solid particles respectively, and can be removed by filtration.
Example 6
The removal of o-, m-and p-methoxyphenols by the heat-activated persulfate system was explored in this example. The experimental parameters were the same as for the heat/PDS/phenol system of example 1, except that the phenol in the heat/PDS/phenol system was replaced. The results show that o-methoxyphenol, m-methoxyphenol and p-methoxyphenol are polymerized in the system to generate dark brown, light brown and light yellow organic solid particles which are removed after precipitation.
Example 7
The effect of thermally activated persulfate systems on the removal of 4-bromophenol was explored in this example. The experimental parameters were the same as for the heat/PDS/phenol system of example 1, except that the phenol was replaced in the heat/PDS/phenol system. The results show that 4-bromophenol is polymerized in the system to generate light brown solid particle precipitate which is removed after standing.
Example 8
The removal of 2-, 3-and 4-chlorophenols by the thermally activated persulfate system was explored in this example. The experimental parameters were the same as for the heat/PDS/phenol system of example 1, except that the phenol in the heat/PDS/phenol system was replaced. The results show that 2-chlorophenol, 3-chlorophenol and 4-chlorophenol undergo polymerization in the system to respectively generate tan, white and earthy yellow solid precipitate substances which are removed from the solution after centrifugation.
Example 9
The removal of terephthalic acid and terephthalic acid by a thermally activated persulfate system was explored in this example. The experimental parameters were the same as for the heat/PDS/phenol system of example 1, except that the phenol in the heat/PDS/phenol system was replaced. The results showed that benzoic acid and terephthalic acid polymerized in the system, both of which formed a yellow organic solid precipitate that was removed from the solution after filtration.
Example 10
The effect of thermally activated persulfate systems on aniline removal was explored in this example. The experimental parameters were the same as for the heat/PDS/phenol system of example 1, except that the phenol in the heat/PDS/phenol system was replaced. The results show that aniline was polymerized in the system to form a reddish brown solid precipitate which can be removed by filtration.
Example 11
The effect of thermally activated persulfate systems on the removal of 2,2 '-dihydroxybiphenyl and 4, 4' -dihydroxybiphenyl was explored in this example. The experimental parameters were the same as for the heat/PDS/phenol system of example 1, except that the phenol was replaced in the heat/PDS/phenol system. The results show that 2,2 '-dihydroxybiphenyl and 4, 4' -dihydroxybiphenyl undergo polymerization in the system to form brown and yellow organic solid precipitates, respectively, and can be removed by filtration.
Example 12
The effect of thermally activated persulfate systems on the removal of 4-nitrophenol was explored in this example. The experimental parameters were the same as for the heat/PDS/phenol system of example 1, except that the phenol in the heat/PDS/phenol system was replaced. The results show that 4-nitrophenol is polymerized in the system to generate fluorescent yellow organic solid precipitate which can be filtered and removed.
Example 13
The effect of thermally activated persulfate systems on the removal of 2, 6-xylenol was explored in this example. The experimental parameters were the same as for the heat/PDS/phenol system of example 1, except that the phenol was replaced in the heat/PDS/phenol system. The results show that 2, 6-xylenol polymerized in the system to form a bright yellow organic solid precipitate which can be removed by filtration.
Example 14
The effect of heat-activated persulfate systems on ascorbic acid removal was explored in this example. The experimental parameters were the same as for the heat/PDS/phenol system of example 1, except that the phenol in the heat/PDS/phenol system was replaced. The results show that ascorbic acid is polymerized in the system to generate a light yellow organic solid precipitate which can be removed after filtration.
Example 15
The removal of o-cresol by a heat-activated persulfate system was explored in this example. The experimental parameters are shown below. The results show that o-cresol polymerizes in the system to form a brown organic solid precipitate which can be removed by filtration.
The specific implementation parameters of the heat/PDS/o-cresol system are as follows:
o-cresol concentration: 1mmol/L
The PDS concentration: 0.5mmol/L
Volume of reaction solution: 200mL
Temperature of the reaction solution: 99 deg.C
pH of the reaction solution: 5
Example 16
The effect of thermally activated persulfate systems on phenol removal was explored in this example. The experimental parameters are shown below. The results show that phenol was polymerized in the system to form a brown organic solid precipitate which can be removed by filtration.
The specific implementation parameters of the heat/PDS/phenol system are as follows:
the phenol concentration: 20mmol/L
The PDS concentration: 1000mmol/L
Volume of reaction solution: 200mL
Temperature of the reaction solution: 40 deg.C
pH of the reaction solution: 5
It will be understood by those skilled in the art that the foregoing is only a preferred embodiment of the present invention, and is not intended to limit the invention, and that any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (8)
1. A method for removing organic pollutants in water by thermally activating persulfate is characterized in that wastewater containing organic pollutants to be treated is used as reaction liquid, the temperature of the reaction liquid is controlled to be above 40 ℃, and persulfate is added into the reaction liquid to carry out reaction; the ratio of the amount of the persulfate to the amount of the organic pollutant in the reaction solution is 0.5-50: 1; in the reaction process, the persulfate can be activated in a thermal environment to generate free radicals, attack organic pollutants to generate organic free radicals, and then perform polymerization reaction to generate organic solid particle precipitates; and (3) carrying out solid-liquid separation on the reaction system after reacting for 3-210 minutes, wherein the liquid obtained by separation is the treated wastewater.
2. The method of claim 1, wherein the persulfate comprises at least one of Peroxymonosulfate (PMS), Peroxydisulfate (PDS); the ratio of the amount of the persulfate to the volume of the reaction solution is preferably 0.5 to 1000 mmol/L.
3. The method of claim 1, wherein when the persulfate comprises Peroxymonosulfate (PMS), the chemical reactions that occur during the reaction include, but are not limited to:
SO4 ·-+ organic contaminants → SO4 2-+ organic solid polymer particles + soluble oxidation products,
HO·+ organic contaminants → HO-+ organic solid polymer particles + soluble oxidation products;
when the persulfate salt comprises a peroxydisulfate salt (PDS), specific chemical reactions that occur during the reaction include, but are not limited to:
SO4 ·-+ organic contaminants → SO4 2-+ organic solid polymer particles + soluble oxidation products,
HO·+ organic contaminants → HO-+ organic solid polymer particles + soluble oxidation products.
4. The method according to claim 1, wherein the temperature of the reaction solution is controlled to 40 to 99 ℃.
5. The method of claim 1, wherein the temperature of the reaction solution is controlled to 40 ℃ or higher by heating, or by directly using high-temperature waste water whose temperature meets the requirement, or by mixing 2 kinds of waste water whose temperature is higher or lower;
the attack organic pollutants attack the organic pollutants by means of addition or hydrogen abstraction or electron transfer.
6. The process according to claim 1, wherein the reaction is preferably carried out under stirring conditions; more preferably, the stirring conditions are achieved by mechanical stirring or aeration stirring.
7. The method according to claim 1, wherein the organic contaminant in the wastewater containing organic contaminants to be treated is one or more of phenolic organic substances, aniline organic substances, alkoxybenzene organic substances, nitrobenzene organic substances, phenolic ester organic substances, benzene or biphenyl organic substances and heterocyclic compounds.
8. The method of claim 1, wherein the solid-liquid separation is achieved by coagulating sedimentation or filtration or centrifugation or static sedimentation.
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