CN108164061B - Method for treating phosphorus-containing and fluorine-containing organic wastewater through microwave wet catalytic oxidation - Google Patents
Method for treating phosphorus-containing and fluorine-containing organic wastewater through microwave wet catalytic oxidation Download PDFInfo
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- C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
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Abstract
The invention discloses a method for treating phosphorus-containing and fluorine-containing organic wastewater by microwave wet catalytic oxidation, which comprises the steps of adjusting the pH value to 2.0-5.0, performing Fenton pretreatment for 2-8h, adjusting the pH value to 7-10 through neutralization reaction, then adjusting the pH value of supernatant after the neutralization reaction to 2.0-6.5 by using sulfuric acid, and adding potassium persulfate with the mass ratio of wastewater after acid adjustment being 0.2-8%; and (3) allowing the wastewater added with the oxidant to enter a microwave reactor for reaction, adding lime into the microwave reaction effluent and the gas condensate for neutralization reaction, allowing the organic wastewater subjected to the neutralization reaction to enter a water storage tank, and adjusting the pH value back to 6-9. The method overcomes the defects of large oxidant dosage and low oxidation efficiency in the traditional oxidation process, and can realize the thorough and effective degradation of the phosphorus-containing and fluorine-containing organic wastewater.
Description
Technical Field
The invention belongs to the field of wastewater treatment, and relates to a method for treating phosphorus-containing fluorine-containing organic wastewater by microwave wet catalytic oxidation.
Background
The fluorine and phosphorus compounds are widely applied to industrial production, particularly the electronic chemical industry, along with the mass construction and production of the electronic industry, the total discharge amount of the fluorine-containing and phosphorus-containing wastewater is increased sharply, some extremely stable fluorine-containing and phosphorus-containing compounds can be generated in the production process, the compounds are not easily oxidized and degraded by the conventional process, and the treatment difficulty is high. Therefore, the invention utilizes Fenton pretreatment combined with a microwave wet catalytic oxidation process to treat the wastewater containing fluorine and phosphorus, and can effectively remove fluorine and phosphorus in the wastewater.
The invention content is as follows:
the invention relates to a method for treating phosphorus-containing and fluorine-containing organic wastewater by microwave wet catalytic oxidation, which adopts Fenton pretreatment combined with microwave wet catalytic oxidation technology. The method for treating the phosphorus-containing and fluorine-containing organic wastewater by utilizing microwave wet catalytic oxidation is characterized by comprising the following operation steps of:
a method for treating phosphorus-containing fluorine-containing organic wastewater by microwave wet catalytic oxidation comprises the following operation steps:
(1) fenton pretreatment: adjusting the pH value of the phosphorus-containing organic wastewater to 2.0-5.0 by using sulfuric acid, adding a Fenton reagent, fully stirring, and reacting for 2-8 hours;
(2) and (3) neutralization reaction: adjusting the pH value of the wastewater subjected to Fenton pre-oxidation to 7-10 by using sodium hydroxide, and standing to obtain a supernatant subjected to neutralization treatment;
(3) acid adjusting treatment: regulating the pH value of the supernatant after the neutralization reaction to 2.0-6.5 by using sulfuric acid;
(4) adding an oxidizing agent: adding potassium persulfate with the mass ratio of 0.2-8% of the wastewater after acid adjustment;
(5) microwave wet catalytic oxidation reaction treatment: the wastewater added with the oxidant enters a microwave reactor for reaction, air is introduced while the reaction is carried out, the air flow is 0.5-2L/min, the microwave power is 150-900W, and the treatment time is 0.5-10 minutes;
(6) and (3) neutralization reaction treatment: the microwave reaction effluent and the gas condensate enter a neutralization reaction sedimentation tank, lime is added for neutralization reaction, the adding amount of the lime is 0.2-4% of the mass of the microwave reaction effluent, and the treatment time is 60-120 minutes; wherein the microwave wet catalytic oxidation exhaust gas is absorbed by an active carbon column;
(7) treating a water storage tank: and (4) allowing the organic wastewater after the neutralization reaction to enter a water storage tank, and adjusting the pH value back to 6-9, wherein the reaction time is 30-60 minutes.
In the technical scheme, preferably, COD (chemical oxygen demand) of the phosphorus-containing organic wastewater to be treated in the step (1) is 500-1000 mg/L, TP is 15-50 mg/L, and F-20-80 mg/L and pH 6-9.
The phosphorus-containing organic wastewater after Fenton pretreatment in the step (1)The COD of the resin is 250-350 mg/L, the TP of the resin is 15-50 mg/L, and F-20-80 mg/L and pH value of 2-5.
The COD of the neutralized phosphorus-containing organic wastewater in the step (2) is 200-300 mg/L, the TP is 15-50 mg/L, and F-20-80 mg/L and pH 7-10.
The COD of the phosphorus-containing organic wastewater treated by the acid adjustment treatment in the step (3) is 200-300 mg/L, the TP is 15-50 mg/L, and F-20-80 mg/L, and a pH value of 2.0-6.5.
After the oxidant is added in the step (4), the COD of the phosphorus-containing organic wastewater is 200-300 mg/L, the TP is 15-50 mg/L, and F-20-80 mg/L and pH of 2.0-6.5.
The COD, TP and F of the phosphorus-containing organic wastewater treated by the microwave wet catalytic oxidation reaction in the step (5) are respectively 35-50 mg/L, 15-50 mg/L and F-20-80 mg/L and pH of 2.0-6.5.
The COD, TP and pH of the organic wastewater subjected to neutralization treatment in the step (6) are respectively 20-30 mg/L, 0-0.5 mg/L and 7.5-10.0.
The COD of the phosphorus-containing organic wastewater treated by the water storage tank in the step (7) is 20-30 mg/L, the TP is 0.1-0.5 mg/L, and F-0.2-4 mg/L and pH 6-9.
The principle of the invention is as follows: when the catalyst is irradiated by high-intensity short-pulse microwaves, the catalyst absorbs the microwaves, the microwave energy is quickly converted into heat, certain surface positions of the catalyst are heated to a high temperature to form microwave hot spots (1200 ℃), pollutants nearby the microwave hot spots are oxidized and degraded at a high temperature, and when an oxidant exists, the microwaves can promote the oxidant to generate OH and high-oxidizing substances.
Compared with the prior art, the invention has the following advantages:
(1) microwave and potassium persulfate are combined, and the potassium persulfate is activated into SO with higher oxidation-reduction potential due to the electromagnetic field effect of the microwave4 2-Can effectively oxidize nitrogen and phosphorus compounds and accelerate the reaction.
(2)O2Can also be used as electron acceptor in microwave wet catalytic oxidation reaction to generate high activity OH, which can accelerate reactionAnd the addition amount of potassium persulfate is reduced.
(3) Potassium persulfate is as strong oxidizing substance, also can oxidize other organic matters in the organic waste water simultaneously, carries out oxidation treatment in advance with fenton and gets rid of most organic matters in the waste water earlier, carries out microwave catalytic oxidation treatment again, can reduce treatment cost by a wide margin.
Drawings
FIG. 1 is a process flow diagram of a method for treating phosphorus-containing and fluorine-containing organic wastewater by microwave wet catalytic oxidation.
Detailed Description
The present invention will be described in further detail with reference to examples, but the embodiments of the present invention are not limited thereto.
A method for treating phosphorus-containing fluorine-containing organic wastewater by microwave wet catalytic oxidation comprises the following operation steps:
(1) fenton pretreatment: adjusting the pH value of the phosphorus-containing organic wastewater to 2.0-5.0 by using sulfuric acid, adding a Fenton reagent, fully stirring, and reacting for 2-8 hours;
(2) and (3) neutralization reaction: adjusting the pH value of the wastewater subjected to Fenton pre-oxidation to 7-10 by using sodium hydroxide, and standing to obtain a supernatant subjected to neutralization treatment;
(3) acid adjusting treatment: regulating the pH value of the supernatant after the neutralization reaction to 2.0-6.5 by using sulfuric acid;
(4) adding an oxidizing agent: adding potassium persulfate with the mass ratio of 0.2-8% of the wastewater after acid adjustment;
(5) microwave wet catalytic oxidation reaction treatment: the wastewater added with the oxidant enters a microwave reactor for reaction, air is introduced while the reaction is carried out, the air flow is 0.5-2L/min, the microwave power is 150-900W, and the treatment time is 0.5-10 minutes;
(6) and (3) neutralization reaction treatment: the microwave reaction effluent and the gas condensate enter a neutralization reaction sedimentation tank, lime is added for neutralization reaction, the adding amount of the lime is 0.2-4% of the mass of the microwave reaction effluent, and the treatment time is 60-120 minutes; wherein the microwave wet catalytic oxidation exhaust gas is absorbed by an active carbon column;
(7) treating a water storage tank: and (4) allowing the organic wastewater after the neutralization reaction to enter a water storage tank, and adjusting the pH value back to 6-9, wherein the reaction time is 30-60 minutes.
Example 1
The method for treating the phosphorus-containing and fluorine-containing organic wastewater by microwave wet catalytic oxidation is adopted for treating certain organic wastewater. COD of an organic wastewater is 850mg/L, TP is 31mg/L, F-48.6mg/L, pH 7.6. Firstly, Fenton pretreatment is carried out, after the Fenton pretreatment, the COD is 258mg/L, the TP is 31mg/L, and F-48.6mg/L, pH 4.2. Adjusting pH of the wastewater after Fenton pre-oxidation to 9.5 with sodium hydroxide, standing to obtain supernatant after neutralization, wherein COD is 205mg/L, TP is 31mg/L, and F is-48.6mg/L, pH9.5. And (3) regulating the pH value of the neutralized supernatant to 4.8 by using sulfuric acid, adding 2g of potassium persulfate, reacting in a microwave reactor, introducing air while reacting, wherein the air flow is 0.5L/min, the microwave power is 500W, and the treatment time is 5 minutes. And (3) allowing the microwave reaction effluent and the gas condensate to enter a neutralization reaction sedimentation tank, adding lime for neutralization reaction, and adding 2.5g of lime for 60 minutes. The microwave wet catalytic oxidation exhaust gas is absorbed by an activated carbon column. At this time, COD was 25mg/L, TP was 0.5, and F-0.2mg/L and a pH of 8.2. The effluent water from the neutralization tank enters a water storage tank and stays for 60 minutes, the TOC of the effluent water is 40mg/L, the COD is 25mg/L, the TP is 0.5, and F-0.2mg/L and a pH of 8.2.
Example 2
The method for treating the phosphorus-containing and fluorine-containing organic wastewater by microwave wet catalytic oxidation is adopted for treating certain organic wastewater. COD of an organic wastewater is 800mg/L, TP is 28mg/L, F-45.5mg/L, pH 7.6. Firstly, Fenton pretreatment is carried out, after the Fenton pretreatment, the COD is 245mg/L, the TP is 28mg/L, and F-45.5mg/L, pH 3.8. Adjusting pH of the wastewater after Fenton pre-oxidation to 9.5 with sodium hydroxide, standing to obtain supernatant after neutralization, wherein COD is 200mg/L, TP is 28mg/L, and F is-45.5mg/L, pH 10. And (3) regulating the pH value of the neutralized supernatant to 5.3 by using sulfuric acid, adding 2g of potassium persulfate, reacting in a microwave reactor, introducing air while reacting, wherein the air flow is 0.5L/min, the microwave power is 500W, and the treatment time is 5 minutes. Micro-meterAnd (3) allowing effluent of the wave reaction and gas condensate to enter a neutralization reaction sedimentation tank, adding lime for neutralization reaction, and adding 2.2g of lime for 60 minutes. The microwave wet catalytic oxidation exhaust gas is absorbed by an activated carbon column. At this time, COD was 20mg/L, TP was 0.3, and F-0.5mg/L and a pH of 8.5. The effluent water from the neutralization tank enters a water storage tank and stays for 60 minutes, the COD of the effluent water is 20mg/L, TP is 0.3, F-0.5 is mg/L, pH 8.5.
Example 3
The method for treating the phosphorus-containing and fluorine-containing organic wastewater by microwave wet catalytic oxidation is adopted for treating certain organic wastewater. COD of an organic wastewater is 816mg/L, TP is 30mg/L, F-47.8mg/L, pH 7.6. Firstly, Fenton pretreatment is carried out, after the Fenton pretreatment, the COD is 223mg/L, the TP is 30mg/L, and F-47.8mg/L, pH 4.0. Adjusting pH of the wastewater after Fenton pre-oxidation to 9.5 with sodium hydroxide, standing to obtain supernatant after neutralization, wherein COD is 201mg/L, TP is 30mg/L, and F is-47.8mg/L, pH 9.5. And (3) regulating the pH value of the neutralized supernatant to 4.3 by using sulfuric acid, adding 2g of potassium persulfate, reacting in a microwave reactor, introducing air while reacting, wherein the air flow is 0.5L/min, the microwave power is 500W, and the treatment time is 5 minutes. And (3) allowing the microwave reaction effluent and the gas condensate to enter a neutralization reaction sedimentation tank, adding lime for neutralization reaction, and adding 2.5g of lime for 60 minutes. The microwave wet catalytic oxidation exhaust gas is absorbed by an activated carbon column. At this time, COD was 22mg/L, TP was 0.5, and F-0.2mg/L and a pH of 8.5. The effluent water from the neutralization tank enters a water storage tank and stays for 60 minutes, the COD of the effluent water is 22mg/L, the TP is 0.5, F-0.2mg/L and a pH of 8.2.
Claims (9)
1. A method for treating phosphorus-containing and fluorine-containing organic wastewater by microwave wet catalytic oxidation is characterized by comprising the following operation steps:
(1) fenton pretreatment: adjusting the pH value of the phosphorus-containing fluorine-containing organic wastewater to 2.0-5.0 by using sulfuric acid, adding a Fenton reagent, fully stirring, and reacting for 2-8 hours;
(2) and (3) neutralization reaction: adjusting the pH value of the wastewater subjected to Fenton pre-oxidation to 7-10 by using sodium hydroxide, and standing to obtain a supernatant subjected to neutralization treatment;
(3) acid adjusting treatment: regulating the pH value of the supernatant after the neutralization reaction to 2.0-6.5 by using sulfuric acid;
(4) adding an oxidizing agent: adding potassium persulfate with the mass ratio of 0.2-8% of the wastewater after acid adjustment;
(5) microwave wet catalytic oxidation reaction treatment: the wastewater added with the oxidant enters a microwave reactor for reaction, air is introduced while the reaction is carried out, the air flow is 0.5-2L/min, the microwave power is 150-900W, and the treatment time is 0.5-10 minutes;
(6) and (3) neutralization reaction treatment: the microwave reaction effluent and the gas condensate enter a neutralization reaction sedimentation tank, lime is added for neutralization reaction, the adding amount of the lime is 0.2-4% of the mass of the microwave reaction effluent, and the treatment time is 60-120 minutes; wherein the microwave wet catalytic oxidation exhaust gas is absorbed by an active carbon column;
(7) treating a water storage tank: and (3) allowing the phosphorus-containing and fluorine-containing organic wastewater after the neutralization reaction to enter a water storage tank, and adjusting the pH value back to 6-9, wherein the reaction time is 30-60 minutes.
2. The method for treating the phosphorus-containing and fluorine-containing organic wastewater by microwave wet catalytic oxidation according to claim 1, wherein the method comprises the following steps: the COD of the phosphorus-containing and fluorine-containing organic wastewater to be treated in the step (1) is 500-1000 mg/L, TP is 15-50 mg/L, F-20-80 mg/L and pH 6-9.
3. The method for treating the phosphorus-containing and fluorine-containing organic wastewater by microwave wet catalytic oxidation according to claim 1, wherein the method comprises the following steps: the COD of the phosphorus-containing and fluorine-containing organic wastewater subjected to Fenton pretreatment in the step (1) is 250-350 mg/L, the TP is 15-50 mg/L, and F-20-80 mg/L and pH value of 2-5.
4. The method for treating the phosphorus-containing and fluorine-containing organic wastewater by microwave wet catalytic oxidation according to claim 1, wherein the method comprises the following steps: the COD of the phosphorus-containing fluorine-containing organic wastewater neutralized in the step (2) is 200-300 mg/L, and the TP is 15-50mg/L，F-20-80 mg/L and pH 7-10.
5. The method for treating the phosphorus-containing and fluorine-containing organic wastewater by microwave wet catalytic oxidation according to claim 1, wherein the method comprises the following steps: after the acid adjustment treatment in the step (3), COD of the phosphorus-containing fluorine-containing organic wastewater is 200-300 mg/L, TP is 15-50 mg/L, and F-20-80 mg/L, and a pH value of 2.0-6.5.
6. The method for treating the phosphorus-containing and fluorine-containing organic wastewater by microwave wet catalytic oxidation according to claim 1, wherein the method comprises the following steps: after the oxidant is added in the step (4), the COD of the phosphorus-containing fluorine-containing organic wastewater is 200-300 mg/L, the TP is 15-50 mg/L, and F-20-80 mg/L and pH of 2.0-6.5.
7. The method for treating the phosphorus-containing and fluorine-containing organic wastewater by microwave wet catalytic oxidation according to claim 1, wherein the method comprises the following steps: the COD, TP and F of the phosphorus-containing and fluorine-containing organic wastewater treated by the microwave wet catalytic oxidation reaction in the step (5) are respectively 35-50 mg/L, 15-50 mg/L and F-20-80 mg/L and pH of 2.0-6.5.
8. The method for treating the phosphorus-containing and fluorine-containing organic wastewater by microwave wet catalytic oxidation according to claim 1, wherein the method comprises the following steps: the COD, TP and pH of the phosphorus-containing and fluorine-containing organic wastewater subjected to neutralization treatment in the step (6) are respectively 20-30 mg/L, 0-0.5 mg/L and 7.5-10.0.
9. The method for treating the phosphorus-containing and fluorine-containing organic wastewater by microwave wet catalytic oxidation according to claim 1, wherein the method comprises the following steps: the COD of the phosphorus-containing fluorine-containing organic wastewater treated by the water storage tank in the step (7) is 20-30 mg/L, the TP is 0.1-0.5 mg/L, and F-0.2-4 mg/L and pH 6-9.
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