CN114906956A - Deep phosphorus removal method for organic phosphorus wastewater adsorbed by microelectrolysis coupling nano composite material - Google Patents
Deep phosphorus removal method for organic phosphorus wastewater adsorbed by microelectrolysis coupling nano composite material Download PDFInfo
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Abstract
The invention discloses a method for deeply removing phosphorus from organophosphorus wastewater adsorbed by a microelectrolysis coupling nano composite material. The invention aims to provide a method for deeply removing total phosphorus in organophosphorus wastewater, wherein the concentration of the total phosphorus in treated effluent is less than or equal to 0.3 mg/L.
Description
Technical Field
The invention relates to advanced treatment of industrial wastewater, in particular to an organophosphorus wastewater advanced phosphorus removal method based on micro-electrolysis coupling nano composite material adsorption.
Background
Phosphorus is an important element in people's life and industrial production, and currently, tens of thousands of organic phosphorus compounds are widely applied, so that the use of the organic phosphorus compounds provides convenience for people's production and life and also causes serious environmental pollution problems. The phosphorus chemical industry in China has large scale, but the overall level is still different from that of developed countries, and the variety of organic phosphorus is wide and is limited by the production technology level and the management level, so that the phosphorus chemical industry in China has the problems of low product recovery rate, more byproducts, large wastewater discharge amount and the like. The phosphorus chemical wastewater has high total phosphorus content, strong toxicity and poor biodegradability, and can not meet the requirements of discharge standards only by adopting the conventional biological treatment technology; once the organic phosphorus wastewater which is not properly treated is discharged into the water body, the problem of water eutrophication can be caused, so that the water quality is rapidly deteriorated, and the sustainable development of the ecological environment is influenced.
The existing treatment method of the organophosphorus wastewater mainly comprises the following steps: biological methods, adsorption methods, cooling crystallization, membrane separation, distillation, extraction, advanced oxidation methods, and the like. The biological method has the defects that toxic and harmful substances in the organophosphorus wastewater can generate irreversible inhibition and toxic action on the activated sludge, so that the treatment effect cannot meet the requirement; the adsorption method has the defects that the concentration of organic matters in the organophosphorus wastewater is high, and the adsorbent is required to be frequently regenerated or updated due to the excessively high adsorption saturation speed of the adsorbent, so that the operation cost is increased; the technologies of cooling crystallization, membrane separation, distillation, extraction and the like can obtain better treatment effect on the organophosphorus wastewater with small flow and higher concentration, but have the defects of complex process flow, high equipment requirement and high treatment cost; the advanced oxidation method is a technology for generating strong oxidative hydroxyl radicals by adopting methods such as light, electricity and chemical reagents to realize the oxidative decomposition of pollutants, and has the advantages of low organic matter selectivity, strong oxidative decomposition capacity, no generation of a large amount of biological sludge and the like.
Iron-carbon microelectrolysis is an advanced oxidation technology which is widely applied, a primary battery can be spontaneously formed by utilizing low-potential Fe ions and high-potential C ions in wastewater to initiate chemical reactions such as oxidation-reduction reaction, flocculation reaction and the like so as to achieve the purpose of removing organic matters, and meanwhile, Fe ions generated by microelectrolysis are hydrolyzed to generate Fe (OH) 3 The flocculating agent can also achieve the effect of chemical precipitation dephosphorization, and is the current methodThe method is an ideal process for treating high-concentration organic phosphorus wastewater, but the treated effluent still contains organic phosphorus which is not oxidized and degraded and inorganic phosphorus which is generated by mineralization and decomposition, so that the Total Phosphorus (TP) concentration of the wastewater cannot meet the discharge requirement, and further treatment is still needed.
Patent document No. 201610141407.5 discloses a method for converting organic phosphorus in organic phosphorus wastewater into inorganic phosphorus, which uses chemical oxidation and solar energy to effectively combine, and uses photocatalytic oxidation technology to convert organic phosphorus in organic phosphorus wastewater into inorganic phosphorus in the form of phosphate, but the patent does not relate to the converted inorganic phosphorus and the further treatment method of the residual non-decomposed organic phosphorus. The patent document with the application number of 201811582881.7 discloses a method for treating high-concentration organic phosphorus wastewater, which adopts an iron-carbon reactor to carry out micro-electrolysis reaction and then adds H 2 O 2 And (3) continuing the reaction, and finally performing flocculation precipitation treatment to realize that the content of organic phosphorus in the treated wastewater is less than or equal to 5 mg/L, but the total phosphorus in the treated wastewater is still higher, so that the requirement of wastewater discharge cannot be met. The patent document with application number 201910802208.8 discloses an "organophosphorus wastewater treatment process" which uses a catalytic oxidation filler to react with active oxygen water to convert organophosphorus in wastewater into phosphate; the clear liquid obtained by the effluent entering a plate-and-frame filter press is pumped into an advanced treatment system filled with resin to adsorb residual phosphorus, so that the content of phosphate in the adsorbed effluent is 0.5 mg/L, but the method has no targeted removal method for residual organic phosphorus after advanced oxidation, and meanwhile, the subsequent resin adsorption lacks selectivity for phosphate adsorption, so that the working period is short, the regeneration is frequent, and the operation cost is high.
In conclusion, the organophosphorus chemical wastewater has the characteristics of high pollutant concentration, complex components, high toxicity, poor biodegradability and the like, so that the efficient and stable standard-reaching treatment of the organophosphorus wastewater is realized, and the problem of the technology in the field is still solved.
Disclosure of Invention
The purpose of the invention is as follows: the invention aims to provide a micro-electrolysis coupling nano composite material adsorption technology for organophosphorus wastewater with high pollutant concentration, complex components, high toxicity and poor biodegradability so as to realize deep removal of total phosphorus in the organophosphorus wastewater.
The technical scheme is as follows: the invention relates to a method for deeply removing phosphorus from organophosphorus wastewater adsorbed by microelectrolysis coupling nano composite material, which comprises the following steps:
(A) the organic phosphorus wastewater is pretreated by a quartz sand filter to filter impurities such as suspended matters in the organic phosphorus wastewater, so that colloidal suspended matters are prevented from being adhered to the surface of a micro-electrolysis filler in a micro-electrolysis reactor, the contact between the iron-carbon micro-electrolysis filler and the organic phosphorus wastewater is hindered, and the micro-electrolysis reaction efficiency is reduced; introducing the organic phosphorus wastewater in the wastewater regulating tank into a quartz sand filter, wherein the quartz sand filter is used for removing suspended pollutants in the wastewater, and filtering by the quartz sand filter to obtain a first filtrate with suspended particulate matters (SS) concentration less than or equal to 10 mg/L;
(B) introducing the first filtrate obtained in the step (A) into a micro-electrolysis reactor, wherein an aerator is arranged in the micro-electrolysis reactor; adding hydrogen chloride (HCl) solution and hydrogen peroxide (H) into a micro-electrolysis reactor 2 O 2 ) Carrying out aeration reaction on the solution for 1.5-3 h to obtain second effluent;
(C) introducing the second effluent obtained in the step (B) into a flocculation reaction tank, wherein a stirring paddle is arranged in the flocculation reaction tank; adding a sodium hydroxide (NaOH) solution, polyferric chloride (PFC) and Polyacrylamide (PAM) into a flocculation reaction tank, and stirring for reaction to obtain a third suspension, wherein the third suspension comprises water and hydroxyl iron phosphate precipitate;
(D) leading the third turbid liquid obtained after the flocculation reaction in the step (C) into a sedimentation tank, arranging an inclined plate in the sedimentation tank, externally connecting a drain pipe at the upper part of the sedimentation tank, externally connecting a sludge discharge pipe at the bottom of the sedimentation tank, and setting the hydraulic load of the sedimentation tank to be 1-3 m 3 /m 2 H, standing the suspension in a sedimentation tank, layering, discharging the supernatant and the hydroxyl iron phosphate precipitate at the lower layer through a drain pipe, discharging the hydroxyl iron phosphate precipitate through a mud discharge pipe, discharging the hydroxyl iron phosphate precipitate every 6-12 h, and purifying the discharged hydroxyl iron phosphate to be comprehensively utilized;
(E) introducing the supernatant obtained in the step (D) into a precision filter, further removing small-particle suspended matters and colloid substances which cannot be separated in a sedimentation tank, and finally obtaining a fifth filtrate of which the concentration of suspended particulate matters (SS) is less than or equal to 5 mg/L and the turbidity is less than or equal to 2 NTU;
(F) introducing the fifth filtrate obtained in the step (E) into an adsorption tower, wherein the adsorption tower is filled with a nano composite phosphorus removal adsorbent for deeply removing residual organic phosphorus and phosphate in the filtrate, and adsorbing to obtain outlet water;
(G) when the effluent TP of the adsorption tower in the step (F) is more than 0.3 mg/L, stopping introducing the fifth filtrate into the adsorption tower, then introducing a sodium hydroxide (NaOH) solution with the concentration of 10% into the adsorption tower, performing desorption regeneration on the nano composite phosphorus removal adsorbent, and refluxing desorption liquid obtained by desorption regeneration to a wastewater adjusting tank; after the desorption is finished, the nano composite dephosphorizing adsorbent is washed by clear water until the pH value of the discharged water is neutral, so that the nano composite dephosphorizing adsorbent can be used for next adsorption.
Furthermore, the nano composite phosphorus removal adsorbent is macroporous cross-linked polyacrylic resin containing a plurality of pore channels, the pore channels are in a cross-linked network structure, and the cross-linked network structure means that the length and the relative position of each pore channel are not specific and are in a state of being interwoven together; the pore canal is internally and fixedly loaded with a plurality of Hydrated Cerium Oxide (HCO) nano particles, the surface of the macroporous cross-linked polyacrylic resin is modified with tertiary amine groups, the Hydrated Cerium Oxide (HCO) nano particles have the function of selectively adsorbing phosphate in the fifth filtrate through hydroxyl ligand exchange, the surface of the macroporous cross-linked polyacrylic resin modified with the tertiary amine groups has the function of adsorbing and removing residual organic phosphorus in the fifth filtrate through micropore filling, electrostatic attraction, hydrogen bonding, pi-pi action and acid-base action, the particle size of the macroporous cross-linked polyacrylic resin is 0.4-0.8 mm, and the pore diameter of the pore canal is 5-50 nm.
Furthermore, the Hydrated Cerium Oxide (HCO) nanoparticles in the pore channels are in a nanocluster shape, the solid loading amount of the Hydrated Cerium Oxide (HCO) nanoparticles is 5-15% (by mass of cerium), and the particle size of the Hydrated Cerium Oxide (HCO) nanoparticles is 10-50 nm.
Further, the tertiary amino is dimethylamine group, and the amino content in each milliliter of macroporous crosslinked polyacrylic resin is more than or equal to 1.2 mmol.
Further, in the step (A), the Chemical Oxygen Demand (COD) of the organophosphorus wastewater in the wastewater regulating tank is 1000-4000 mg/L, the concentration of TP is 50-400 mg/L, the particle size of quartz sand in the quartz sand filter is 0.5-1.2 mm, and the filtering speed is 6-12 m/h.
Further, in the step (B), the micro-electrolysis reactor is filled with an iron-carbon micro-electrolysis filler, the iron content of the iron-carbon micro-electrolysis filler is more than or equal to 70 percent, the carbon content of the iron-carbon micro-electrolysis filler is more than or equal to 20 percent, and the volume of the iron-carbon micro-electrolysis filler is 60 to 70 percent of the volume of the micro-electrolysis reactor; the concentration of a hydrogen chloride (HCl) solution added into the micro-electrolysis reactor is 10%, and the hydrogen chloride (HCl) solution is used for adjusting the pH of the organic phosphorus wastewater to 1-3; the concentration of the hydrogen peroxide solution added into the micro-electrolysis reactor is 30%, and the adding amount of the hydrogen peroxide is 4-10 mL per liter of the first filtrate; fe produced during iron-carbon micro-electrolysis reaction 2+ Can catalyze hydrogen peroxide (H2O 2) to generate hydroxyl radical (i.e., -OH), so that organic phosphorus in the first filtrate is oxidized and decomposed into phosphate and CO 2 And H 2 Inorganic substances such as O; the aerator in the micro-electrolysis reactor is a microporous aeration disc and is arranged at the bottom of the micro-electrolysis reactor, the diameter of an air hole of the microporous aeration disc is less than or equal to 2 mm, and the volume ratio of aeration quantity to the first filtrate is 4-10: 1.
Further, the concentration of the sodium hydroxide (NaOH) solution added in the step (C) is 10%, and the sodium hydroxide (NaOH) solution is used for adjusting the pH value of the second effluent to 5-6; adding the polyferric chloride (PFC) and the Polyacrylamide (PAM) in a wet adding manner (wet adding is a common term in the industry, namely firstly dissolving an added substance in water to form an added substance solution, and then adding the added substance solution into the added liquid), wherein the concentration of the polyferric chloride (PFC) solution is 5-10%, and the adding amount is 2-10 mg per liter of second effluent; the concentration of the Polyacrylamide (PAM) solution is 0.2-0.3%, and the addition amount is 0.1-0.5 mg per liter of second effluent; the stirring paddle is firstly used for quickly stirring for 1-3 minutes at the speed of 150-300 revolutions per minute and then is used for slowly stirring for 15-30 minutes at the rotating speed of 30-60 revolutions per minute.
Further, the filter element of the precision filter in the step (E) is a polypropylene melt-blown filter element, and the filtering precision of the precision filter is 1-5 μm.
Further, in the step (F), the flow direction of the fifth filtrate in the adsorption tower is from top to bottom, and the flow speed of the fifth filtrate in the adsorption tower is 3-5 BV (volume of the adsorption bed layer)/h.
Further, in the step (G), the flow direction of the sodium hydroxide (NaOH) solution in the adsorption tower is from top to bottom, the concentration of the sodium hydroxide (NaOH) solution is 10%, and the flow rate of the sodium hydroxide (NaOH) solution is 0.5-1 BV (volume of the adsorption bed layer)/h.
Has the advantages that: compared with the prior art, the invention has the following remarkable advantages:
1. after iron-carbon microelectrolysis and flocculation precipitation reaction, organic phosphorus which is not oxidized and decomposed and phosphate which is not removed by flocculation precipitation are inevitably remained in the obtained fifth filtrate, and the requirement of standard discharge cannot be met. The method adopts an adsorption tower filled with a nano-composite phosphorus removal adsorbent to further adsorb and remove the residual total phosphorus in the organophosphorus wastewater, the nano-composite phosphorus removal adsorbent is coupled with the performance of selective adsorption on phosphate and the high-efficiency adsorption performance on organophosphorus, and the concentration of the total phosphorus in the effluent obtained after adsorption treatment is less than or equal to 0.3 mg/L, so that the total phosphorus can reach the IV-class water standard in the environmental quality Standard of surface Water (GB 3838-2002);
2. the nano composite dephosphorizing adsorbent has high mechanical strength, excellent organic pollution resistance and good regeneration performance, can be repeatedly used for a long time after desorption and regeneration, and reduces the operation cost of enterprises;
3. hydrogen peroxide is added in the micro-electrolysis reaction, and Fe generated by iron-carbon micro-electrolysis can be utilized 2+ Catalyzing hydrogen peroxide to generate hydroxyl radicals, so that organic phosphorus is oxidized and decomposed into inorganic matters such as phosphate and the like; meanwhile, the micro-electrolysis reaction is controlled to be carried out under the acidic condition, so that the electrode reaction of iron and carbon can be accelerated, and Fe can be promoted 2+ The dissolution enhances the catalytic action on hydrogen peroxide, is beneficial to generating more hydroxyl radicals and enhances the oxidative decomposition action on organic phosphorus;
4. iron ions generated by the micro-electrolysis reaction can continue to generate the flocculation reaction in the environment with the increased pH value, so that the consumption of PFC in the flocculation reaction can be saved to a certain extent.
In conclusion, the method has the advantages of simple operation process and low operation cost, the standard treatment of the organophosphorus wastewater can be realized after the method is used, the obtained hydroxyl ferric phosphate precipitate can be comprehensively utilized after being purified, and the environmental benefit and the economic benefit are generated simultaneously.
Drawings
FIG. 1 is a process flow diagram of the present invention;
FIG. 2 is a schematic structural diagram of the nanocomposite phosphorus removal adsorbent of the present invention.
Wherein: 1. a wastewater adjusting tank; 2. a quartz sand filter; 3. a micro-electrolysis reactor; 31. a microporous aeration disc; 4. a flocculation reaction tank; 41. a stirring paddle; 5. a sedimentation tank; 6. a precision filter; 7. an adsorption tower; 8. a nano-composite dephosphorizing adsorbent; 81. macroporous cross-linked polyacrylic resin; 82. a duct; 83. hydrated cerium oxide nanoparticles; 84. dimethylamine groups.
Detailed Description
Example 1
Introducing the organophosphorus wastewater with COD of 1850 mg/L, TP of 162 mg/L in the wastewater regulating tank 1 into a quartz sand filter 2 to remove suspended pollutants in the wastewater; the particle size of the quartz sand is 0.8 mm, the filtering speed is controlled to be 8 m/h, and first filtrate with SS less than or equal to 10 mg/L is obtained; the first filtrate is led into a micro-electrolysis reactor 3, iron-carbon micro-electrolysis filler with iron content more than or equal to 70 percent and carbon content more than or equal to 20 percent is filled in the micro-electrolysis reactor 3, and the volume of the iron-carbon micro-electrolysis filler is 65 percent of the effective volume of the micro-electrolysis reactor 3; adding 10% HCl solution to adjust the pH value of the first filtrate to 2 +/-0.2, and adding 30% hydrogen peroxide solution by mass fraction according to the adding amount of 7 mL/L; the bottom of the micro-electrolysis reactor 3 is aerated by adopting a microporous aeration disc 31, the diameter of the bubbles is less than or equal to 2 mm, and the volume ratio of aeration rate to the first filtrate is 6: and 1, carrying out aeration reaction for 2 h to oxidize and decompose organic phosphorus in the first filtrate into inorganic matters such as phosphate and the like to obtain second effluent.
The second effluent is led into a flocculation reaction tank 4, and 10 percent of NaOH solution is added to adjust the p of the second effluentH, adding 5% of a polyferric chloride (PFC) solution according to the addition amount of 4 mg/L, and adding 0.25% of a Polyacrylamide (PAM) solution according to the addition amount of 0.3 mg/L; stirring paddles 41 in the reaction tank are firstly stirred rapidly for 2 minutes at a speed of 200 revolutions per minute and then stirred slowly for 20 minutes at a rotating speed of 40 revolutions per minute to obtain a third suspension; introducing the third suspension into a sedimentation tank 5, arranging an inclined plate in the sedimentation tank 5, wherein the flow direction of the third suspension in the sedimentation tank 5 is from bottom to top, and the hydraulic load of the sedimentation tank 5 is 2 m 3 /m 2 H, after layering, taking supernatant as the upper layer, taking hydroxyl iron phosphate precipitate as the lower layer, discharging the supernatant through a drain pipe at the upper part of the sedimentation tank 5, discharging the hydroxyl iron phosphate precipitate through a mud pipe at the bottom, and discharging the hydroxyl iron phosphate precipitate once every 8 h, wherein the hydroxyl iron phosphate precipitate can be comprehensively utilized after being purified; and (3) introducing the supernatant into a precision filter 6, further removing unseparated small-particle suspended matters and colloid substances in the supernatant by adopting a polypropylene melt-blown filter element with the filtering precision of 5 mu m, and obtaining a fifth filtrate with SS (suspended solid) less than or equal to 5 mg/L and turbidity less than or equal to 2 NTU.
Introducing the fifth filtrate into an adsorption tower 7, wherein the adsorption tower 7 is filled with a nano composite phosphorus removal adsorbent 8 for deeply removing residual organic phosphorus and phosphate in the fifth filtrate; the nano-composite dephosphorizing adsorbent 8 is macroporous crosslinked polyacrylic resin 81 with a plurality of crosslinked network-shaped pore canals 82 arranged inside, the particle size of the macroporous crosslinked polyacrylic resin 81 is 0.8 mm, and the specific surface area is 600 m 2 The hydrated cerium oxide nanoparticles 83 are fixed in the pore channels 82 in the form of nanoclusters, the solid loading is 10% (mass percentage, calculated by cerium), and the particle size of the hydrated cerium oxide nanoparticles 83 is 30 nm; the surface of the macroporous crosslinked polyacrylic resin 81 is modified with dimethylamine 84, the content of amino in each milliliter of the macroporous crosslinked polyacrylic resin 81 is more than or equal to 1.2 mmol, and the fifth filtrate passes through the nano-composite phosphorus removal adsorbent 8 from top to bottom at the flow rate of 4 BV/h, so that the TP of the adsorbed effluent is less than or equal to 0.3 mg/L; when the TP of the effluent of the adsorption tower 7 is more than 0.3 mg/L, the adsorption is stopped, NaOH solution with the concentration of 10 percent is introduced into the adsorption tower 7, the NaOH solution passes through the nano-composite phosphorus removal adsorbent 8 from top to bottom at the flow rate of 1 BV/h, the desorption regeneration is carried out on the nano-composite phosphorus removal adsorbent 8, and the obtained desorption solution flows back to the wastewater adjusting tank 1. Is desorbed completelyAfter the formation, the nanocomposite phosphorus removal adsorbent 8 is washed with clear water until the effluent is neutral, so that the nanocomposite phosphorus removal adsorbent 8 can be used for the next adsorption operation.
Example 2
Introducing organophosphorus wastewater with COD of 1020 mg/L and TP of 54 mg/L in the wastewater regulating tank 1 into a quartz sand filter 2 to remove suspended pollutants in the wastewater; the particle size of the quartz sand is 1.2 mm, the filtering speed is controlled to be 12 m/h, and first filtrate with SS less than or equal to 10 mg/L is obtained; the first filtrate is led into a micro-electrolysis reactor 3, iron-carbon micro-electrolysis filler with iron content more than or equal to 70 percent and carbon content more than or equal to 20 percent is filled in the micro-electrolysis reactor 3, and the volume of the iron-carbon micro-electrolysis filler is 60 percent of the effective volume of the micro-electrolysis reactor 3; adding 10% HCl solution to adjust the pH value of the first filtrate to 2.8 +/-0.2, and adding 30% hydrogen peroxide solution by mass fraction according to the adding amount of 4 mL/L; the bottom of the micro-electrolysis reactor 3 is aerated by adopting a microporous aeration disc 31, the diameter of bubbles is less than or equal to 2 mm, and the volume ratio of aeration rate to the first filtrate is 4: and 1, carrying out aeration reaction for 1.5 h to oxidize and decompose organic phosphorus in the first filtrate into inorganic matters such as phosphate and the like to obtain second effluent.
Introducing the second effluent into a flocculation reaction tank 4, adding 10% NaOH solution to adjust the pH of the second effluent to 5-6, adding 10% of Polymeric Ferric Chloride (PFC) solution according to the addition amount of 2 mg/L, and adding 0.2% of Polyacrylamide (PAM) solution according to the addition amount of 0.15 mg/L; stirring paddles 41 in the reaction tank are firstly stirred rapidly for 1 minute at the speed of 300 revolutions per minute and then stirred slowly for 15 minutes at the rotating speed of 60 revolutions per minute to obtain a third suspension; introducing the third suspension into a sedimentation tank 5, arranging an inclined plate in the sedimentation tank 5, wherein the flow direction of the third suspension in the sedimentation tank 5 is from bottom to top, and the hydraulic load of the sedimentation tank 5 is 3 m 3 /m 2 H, after layering, taking supernatant as the upper layer, taking hydroxyl iron phosphate precipitate as the lower layer, discharging the supernatant through a drain pipe at the upper part of the sedimentation tank 5, discharging the hydroxyl iron phosphate precipitate through a mud pipe at the bottom, and discharging the hydroxyl iron phosphate precipitate once every 12 h, wherein the hydroxyl iron phosphate precipitate can be comprehensively utilized after being purified; introducing the supernatant into a precision filter 6, adopting a polypropylene melt-blown filter element with the filtering precision of 5 mu m, further removing unseparated small-particle suspended matters and colloid substances in the supernatant to obtain the product with the SS less than or equal to5 mg/L and turbidity less than or equal to 2 NTU.
Introducing the fifth filtrate into an adsorption tower 7, wherein the adsorption tower 7 is filled with a nano composite phosphorus removal adsorbent 8 for deeply removing residual organic phosphorus and phosphate in the fifth filtrate; the nano-composite dephosphorizing adsorbent 8 is macroporous crosslinked polyacrylic resin 81 with a plurality of crosslinked network-shaped pore canals 82 arranged inside, the particle size of the macroporous crosslinked polyacrylic resin 81 is 1.2 mm, and the specific surface area is 500 m 2 The hydrated cerium oxide nanoparticles 83 are fixed in the pore channels 82 in the form of nanoclusters, the solid loading is 5% (mass percentage, calculated by cerium), and the particle size of the hydrated cerium oxide nanoparticles 83 is 50 nm; the surface of the macroporous crosslinked polyacrylic resin 81 is modified with dimethylamine 84, the content of amino in each milliliter of the macroporous crosslinked polyacrylic resin 81 is more than or equal to 1.2 mmol, and the fifth filtrate passes through the nano-composite phosphorus removal adsorbent 8 from top to bottom at the flow rate of 5 BV/h, so that the TP of the adsorbed effluent is less than or equal to 0.3 mg/L; when the TP of the effluent of the adsorption tower 7 is more than 0.3 mg/L, the adsorption is stopped, NaOH solution with the concentration of 10 percent is introduced into the adsorption tower 7, the NaOH solution passes through the nano-composite phosphorus removal adsorbent 8 from top to bottom at the flow rate of 1 BV/h, the desorption regeneration is carried out on the nano-composite phosphorus removal adsorbent 8, and the obtained desorption solution flows back to the wastewater adjusting tank 1. After the desorption is completed, the nanocomposite phosphorus removal adsorbent 8 is washed with clear water until the effluent is neutral, so that the nanocomposite phosphorus removal adsorbent 8 can be used for the next adsorption operation.
Example 3
Introducing organophosphorus wastewater with COD of 3940 mg/L and TP of 385 mg/L in the wastewater regulating tank 1 into a quartz sand filter 2 to remove suspended pollutants in the wastewater; the particle size of the quartz sand is 0.5 mm, the filtering speed is controlled to be 6 m/h, and first filtrate with SS less than or equal to 10 mg/L is obtained; introducing the first filtrate into a micro-electrolysis reactor 3, wherein iron-carbon micro-electrolysis filler with the iron content of more than or equal to 70 percent and the carbon content of more than or equal to 20 percent is filled in the micro-electrolysis reactor 3, and the volume of the iron-carbon micro-electrolysis filler is 70 percent of the effective volume of the micro-electrolysis reactor 3; adding 10% HCl solution to adjust the pH value of the first filtrate to 1.2 +/-0.2, and adding 30% hydrogen peroxide solution by mass fraction according to the adding amount of 10 mL/L; the bottom of the micro-electrolysis reactor 3 is aerated by adopting a microporous aeration disc 31, the diameter of bubbles is less than or equal to 2 mm, and the volume ratio of aeration rate to the first filtrate is 10: and 1, carrying out aeration reaction for 3 hours to oxidize and decompose organic phosphorus in the first filtrate into inorganic matters such as phosphate and the like to obtain second effluent.
Introducing the second effluent into a flocculation reaction tank 4, adding 10% NaOH solution to adjust the pH of the second effluent to 5-6, adding 10% Polymeric Ferric Chloride (PFC) solution according to the adding amount of 10 mg/L, and adding 0.3% Polyacrylamide (PAM) solution according to the adding amount of 0.3 mg/L; stirring paddles 41 in the reaction tank are firstly stirred at a speed of 150 revolutions per minute for 3 minutes and then at a slow speed of 30 revolutions per minute for 30 minutes to obtain a third suspension; introducing the third suspension into a sedimentation tank 5, arranging an inclined plate in the sedimentation tank 5, wherein the flow direction of the third suspension in the sedimentation tank 5 is from bottom to top, and the hydraulic load of the sedimentation tank 5 is 1 m 3 /m 2 H, after layering, taking supernatant as the upper layer, taking hydroxyl iron phosphate precipitate as the lower layer, discharging the supernatant through a drain pipe at the upper part of the sedimentation tank 5, discharging the hydroxyl iron phosphate precipitate through a mud pipe at the bottom, and discharging the hydroxyl iron phosphate precipitate once every 6 h, wherein the hydroxyl iron phosphate precipitate can be comprehensively utilized after being purified; and (3) introducing the supernatant into a precision filter 6, further removing unseparated small-particle suspended matters and colloid substances in the supernatant by adopting a polypropylene melt-blown filter element with the filtering precision of 1 mu m, and obtaining a fifth filtrate with SS (suspended solid) less than or equal to 5 mg/L and turbidity less than or equal to 2 NTU.
Introducing the fifth filtrate into an adsorption tower 7, wherein the adsorption tower 7 is filled with a nano composite phosphorus removal adsorbent 8 for deeply removing residual organic phosphorus and phosphate in the fifth filtrate; the nano-composite dephosphorizing adsorbent 8 is macroporous crosslinked polyacrylic resin 81 with a plurality of pore channels 82 arranged inside, the particle size of the macroporous crosslinked polyacrylic resin 81 is 0.5 mm, and the specific surface area is 700 m 2 The hydrated cerium oxide nanoparticles 83 are fixed in the pore channels 82 in the form of nanoclusters, the solid loading is 15% (mass percentage, calculated by cerium), and the particle size of the hydrated cerium oxide nanoparticles 83 is 10 nm; the surface of the macroporous crosslinked polyacrylic resin 81 is modified with dimethylamine 84, the content of amino in each milliliter of the macroporous crosslinked polyacrylic resin 81 is more than or equal to 1.2 mmol, and the fifth filtrate passes through the nano-composite phosphorus removal adsorbent 8 from top to bottom at the flow rate of 3 BV/h, so that the TP of the adsorbed effluent is less than or equal to 0.3 mg/L; stopping adsorption when the TP of the effluent of the adsorption tower 7 is more than 0.3 mg/L, and then introducingNaOH solution with the concentration of 10% is introduced into the adsorption tower 7, the NaOH solution passes through the nano composite phosphorus removal adsorbent 8 from top to bottom at the flow rate of 0.5 BV/h, desorption regeneration is carried out on the nano composite phosphorus removal adsorbent 8, and the obtained desorption solution flows back to the wastewater adjusting tank 1. After the desorption is completed, the nanocomposite phosphorus removal adsorbent 8 is washed with clear water until the effluent is neutral, so that the nanocomposite phosphorus removal adsorbent 8 can be used for the next adsorption operation.
Claims (10)
1. The deep phosphorus removal method of the organic phosphorus wastewater absorbed by the micro-electrolysis coupling nano composite material comprises the following steps:
(A) introducing the organic phosphorus wastewater in the wastewater regulating tank (1) into a quartz sand filter (2), and filtering the organic phosphorus wastewater by the quartz sand filter (2) to obtain a first filtrate with the concentration of suspended particulate matters (SS) less than or equal to 10 mg/L;
(B) introducing the first filtrate obtained in the step (A) into a micro-electrolysis reactor (3), wherein an aerator is arranged in the micro-electrolysis reactor (3); adding a hydrogen chloride solution and a hydrogen peroxide solution into the micro-electrolysis reactor (3), and carrying out aeration reaction for 1.5-3 h to obtain second effluent;
(C) introducing the second effluent obtained in the step (B) into a flocculation reaction tank (4), wherein a stirring paddle is arranged in the flocculation reaction tank (4); adding a sodium hydroxide solution, polyferric chloride and polyacrylamide into the flocculation reaction tank (4), and stirring for reaction to obtain a third suspension;
(D) introducing the third suspension obtained by the flocculation reaction in the step (C) into a sedimentation tank (5), wherein an inclined plate is arranged in the sedimentation tank (5), the upper part of the sedimentation tank (5) is externally connected with a drain pipe, and the lower part or the bottom of the sedimentation tank (5) is externally connected with a sludge discharge pipe; the hydraulic load of the sedimentation tank is 1-3 m 3 /m 2 H, standing the suspension in a sedimentation tank (5) and then layering, wherein the upper layer is supernatant, the lower layer is hydroxyl iron phosphate precipitate, the supernatant is discharged through a drain pipe, the hydroxyl iron phosphate precipitate is discharged through a mud pipe, and the hydroxyl iron phosphate precipitate is discharged every 6-12 h;
(E) introducing the supernatant obtained in the step (D) into a precision filter (6) to obtain a fifth filtrate of which the concentration of suspended particulate matters (SS) is less than or equal to 5 mg/L and the turbidity is less than or equal to 2 NTU;
(F) introducing the fifth filtrate obtained in the step (E) into an adsorption tower (7), wherein the adsorption tower (7) is filled with a nano-composite phosphorus removal adsorbent (8), and adsorbing to obtain effluent;
(G) when the effluent TP of the adsorption tower (7) in the step (F) is more than 0.3 mg/L, stopping introducing the fifth filtrate into the adsorption tower (7), then introducing a sodium hydroxide solution into the adsorption tower (7) to perform desorption regeneration on the nano composite phosphorus removal adsorbent, and refluxing desorption liquid obtained by desorption regeneration to a wastewater adjusting tank (1); after the desorption is finished, the nano composite phosphorus removal is washed by clear water until the pH value of the effluent is neutral.
2. The method for deeply removing phosphorus from organophosphorus wastewater adsorbed by microelectrolytic coupling nano composite material according to claim 1, is characterized in that: the nano composite phosphorus removal adsorbent (8) is macroporous cross-linked polyacrylic resin (81) containing a plurality of pore channels (82), the pore channels (82) are in a cross-linked network structure, and a plurality of hydrated cerium oxide nano particles (83) are fixedly loaded in the pore channels (82); the surface of the macroporous crosslinked polyacrylic resin (81) is modified with tertiary amine groups, the particle size of the macroporous crosslinked polyacrylic resin (81) is 0.4-0.8 mm, and the pore diameter of the pore channel (82) is 5-50 nm.
3. The method for deeply removing phosphorus from organophosphorus wastewater adsorbed by microelectrolytic coupling nano composite material according to claim 2, which is characterized by comprising the following steps of: the hydrated cerium oxide nanoparticles (83) in the pore channels (82) are in a nanocluster shape, the solid loading of the hydrated cerium oxide nanoparticles (83) is 5-15% (by mass of cerium), and the particle size of the hydrated cerium oxide nanoparticles (83) is about 10-50 nm.
4. The method for deeply removing phosphorus from organophosphorus wastewater adsorbed by microelectrolytic coupling nanocomposite material according to claim 2 or 3, wherein the method comprises the following steps: the tertiary amino is dimethylamine group (84), and the amino content in each milliliter of macroporous crosslinked polyacrylic resin (81) is more than or equal to 1.2 mmol.
5. The method for deeply removing phosphorus from organophosphorus wastewater adsorbed by microelectrolytic coupling nano composite material according to claim 1, is characterized in that: in the step (A), the COD of the organophosphorus wastewater in the wastewater regulating tank (1) is 1000-4000 mg/L, the concentration of TP is 50-400 mg/L, the particle size of quartz sand in the quartz sand filter (2) is 0.5-1.2 mm, and the filtering speed is 6-12 m/h.
6. The method for deeply removing phosphorus from organophosphorus wastewater adsorbed by microelectrolytic coupling nano composite material according to claim 1, is characterized in that: in the step (B), the micro-electrolysis reactor (3) is filled with an iron-carbon micro-electrolysis filler, the iron content of the iron-carbon micro-electrolysis filler is more than or equal to 70 percent, the carbon content of the iron-carbon micro-electrolysis filler is more than or equal to 20 percent, and the volume of the iron-carbon micro-electrolysis filler is 60 to 70 percent of the volume of the micro-electrolysis reactor (3); the concentration of the hydrogen chloride solution added into the micro-electrolysis reactor (3) is 10 percent, and the hydrogen chloride solution is used for adjusting the pH value of the organic phosphorus wastewater to 1-3; the concentration of a hydrogen peroxide solution added into the micro-electrolysis reactor (3) is 30%, and the adding amount of the hydrogen peroxide is 4-10 mL per liter of the first filtrate; the aerator in the micro-electrolysis reactor (3) is a microporous aeration disc (31) and is arranged at the bottom of the micro-electrolysis reactor (3), the diameter of an air hole of the microporous aeration disc (31) is less than or equal to 2 mm, and the volume ratio of aeration quantity to first filtrate is 4-10: 1.
7. the method for deeply removing phosphorus from organophosphorus wastewater adsorbed by microelectrolytic coupling nano composite material according to claim 1, is characterized in that: the concentration of the sodium hydroxide solution in the step (C) is 10%, and the pH of the second effluent is adjusted to 5-6 by the sodium hydroxide solution; the adding mode of the polyferric chloride and the polyacrylamide is wet adding, the concentration of a polyferric chloride solution is 5-10%, the adding amount is 2-10 mg per liter of second effluent, the concentration of a polyacrylamide solution is 0.2-0.3%, and the adding amount is 0.1-0.5 mg per liter of second effluent; a stirring paddle (41) is arranged in the flocculation reaction tank (4), the stirring paddle (41) is firstly quickly stirred for 1-3 minutes at the speed of 150-300 revolutions per minute, and then is slowly stirred for 15-30 minutes at the rotating speed of 30-60 revolutions per minute.
8. The method for deeply removing phosphorus from organophosphorus wastewater adsorbed by microelectrolytic coupling nano composite material according to claim 1, is characterized in that: in the step (E), the filter element of the precision filter (6) is a polypropylene melt-blown filter element, and the filtering precision of the precision filter (6) is 1-5 mu m.
9. The method for deeply removing phosphorus from organophosphorus wastewater adsorbed by microelectrolytic coupling nano composite material according to claim 1, is characterized in that: and (F) enabling the flow direction of the fifth filtrate in the adsorption tower (7) to be from top to bottom, and enabling the flow speed of the fifth filtrate in the adsorption tower (7) to be 3-5 BV/h.
10. The method for deeply removing phosphorus from organophosphorus wastewater adsorbed by microelectrolytic coupling nano composite material according to claim 1, is characterized in that: in the step (G), the flow direction of the sodium hydroxide solution in the adsorption tower (7) is from top to bottom, the concentration of the sodium hydroxide solution is 10%, and the flow rate of the sodium hydroxide solution is 0.5-1 BV/h.
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