CN101905933A - Treating method for phosphoric waste water and sludge generated in production process of phosphatic compound fertilizer - Google Patents
Treating method for phosphoric waste water and sludge generated in production process of phosphatic compound fertilizer Download PDFInfo
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- CN101905933A CN101905933A CN 201010239439 CN201010239439A CN101905933A CN 101905933 A CN101905933 A CN 101905933A CN 201010239439 CN201010239439 CN 201010239439 CN 201010239439 A CN201010239439 A CN 201010239439A CN 101905933 A CN101905933 A CN 101905933A
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Abstract
The invention discloses a treating method for phosphoric waste water and sludge generated in the production process of a phosphatic compound fertilizer, which comprises the following steps: adding lime milk into the phosphoric waste water to be treated firstly, and controlling a pH value to be 5-6; carrying out neutralization reaction for the first time; adding a PAM flocculating agent for flocculation reaction and then carrying out separation of mud and water; adding the lime milk in the aqueous phase again, and controlling the pH value to be 10-11 for the neutralization reaction for the second time; and adding the PAM flocculating agent again for the flocculation reaction and then carrying out the separation of mud and water, wherein the aqueous phase reaches a effluent standard after filtration. The invention realizes the multiplexing or the standard-reaching discharge of the waste water, the zero release of the sludge, accords to the developing direction of the energy saving and emission reduction and circular economy. The clear liquid treated by the process of the invention contains 0.4-0.5mg/L of phosphate (calculated by being based on P2O5), 8-9mg/L of F and 60-80mg/L of COD, meets the primary standard emission requirement of GB8978-1996, the ultimate clear liquid can be returned to a phosphoric acid device for multiplexing, and also be directly discharged after reaching standards; and the sludge produced by the filtration comprises the following main components: calcium phosphate, calcium fluoride, calcium carbonate and calcium sulfate, which can be totally reused as phosphorite resources.
Description
Technical field
The invention belongs to the treatment process of phosphorus-containing wastewater and sludge, specifically, relate to the phosphorus-containing wastewater that produces in the multiple fertile production process of a kind of special disposal phosphorus and the treatment process of sludge.
Background technology
Treatment of Phosphorus Containing Waste Water technology is more, mainly is divided into chemical dephosphorization method and biological phosphate-eliminating method, and the chemical dephosphorization method is used comparatively extensive, and dephosphorization is more thorough, and operational management is easy, and Operation and Maintenance is easy; The biological phosphate-eliminating method is stable, and phosphor-removing effect is good, but for the trade effluent that produces in the multiple fertile production process of phosphorus, lacks necessary carbon source and the nitrogenous source of microorganism growth in the water, if use this method, then needs to add relatively large carbon and nitrogen, the microbial acclimation difficulty.Therefore, the industrial phosphorus-containing wastewater treatment method is mainly chosen in chemical method.
Phosphorus in the trade effluent exists with the form of inorganic phosphorus, and the method that belongs to chemical dephosphorization has: coagulating sedimentation dephosphorization technique and crystallization dephosphorization technique.Crystallization is used less, and reaction conditions is wayward.The coagulating sedimentation dephosphorization technique is divided into metal-salt coagulating sedimentation dephosphorization technique and lime coagulation dephosphorization technique again, and is in the majority with aluminium salt in metal-salt coagulating sedimentation dephosphorization technique.The handling principle of two kinds of treatment process is identical, and phosphor-removing effect is good.It is extensive that lime has raw material sources, cheap advantage, but treatment system is complicated, and the quantity of slag of generation is big; Aluminium salt technology is invested and economized, and the operation operation is easy, and is difficult but cost of material is higher relatively, the waste residue of generation is recycled.
The present invention overcomes treatment system complexity in the traditional technology, shortcomings such as the quantity of slag that produces is big adopt the neutralization of secondary lime, the dense precipitator method of secondary highly effective coagulation, sludges such as the calcium phosphate of generation, Calcium Fluoride (Fluorspan), lime carbonate and calcium sulfate, after mummification, do the phosphate rock resource reuse, realize the zero release of sludge.The industry development direction that meets energy-saving and emission-reduction, resource circulation utilization.
Summary of the invention
For solving above technical problem, the object of the present invention is to provide a kind of technology simple, discharge of wastewater is up to standard, and sludge is recycled the phosphorus-containing wastewater that produces in the multiple fertile production process of the phosphorus reach zero release and the treatment process of sludge.
The present invention seeks to realize like this:
The phosphorus-containing wastewater that produces in the multiple fertile production process of a kind of phosphorus and the treatment process of sludge, carry out according to the following steps: pending phosphorus-containing wastewater adds milk of lime earlier, control pH value 5～6 is carried out the neutralization reaction first time, adds the PAM flocculation agent then and carries out mud-water separation after the flocculation reaction; Water adds milk of lime once more, and control pH value 10～11 is carried out the neutralization reaction second time, adds the PAM flocculation agent once more and carries out mud-water separation after the flocculation reaction, and water reaches emission standard after filtering.
In conjunction with the characteristic of phosphoric acid salt in the waste water and fluorochemical, by adding neutralizing agent milk of lime and PAM flocculation agent etc., a series of neutralization, flocculation reaction take place, dephosphorization simultaneously and defluorination kill two birds with one stone.For strengthening dephosphorization, defluorination effect, adopt the neutralization of secondary lime, the dense precipitating process of secondary highly effective coagulation.This technology dephosphorization and defluorination effect are all better, and clear liquid can return the multiplexing or qualified discharge of phosphoric acid plant, and press filtration produces waste residue and is mainly calcium phosphate, Calcium Fluoride (Fluorspan), lime carbonate and calcium sulfate, as the phosphate rock resource reuse, meets the principle of recycling economy.And raw material is cheap, and working cost is low.
Specifically carry out as follows:
(a) the phosphorus-containing wastewater metering adds milk of lime after pump is squeezed into I level neutralization reaction pond, pH value 5～6 in the control flume, and control air-flow stirring velocity is 5L/min, makes waste water be the milkiness shape, fully reacts 25～30min;
(b) add the PAM flocculation agent to one-level neutralization reaction slip, mixed solution is squeezed into the dense precipitation machine of I level highly effective coagulation through pump;
(c) the upper clear supernate overflow enters II level neutralization reaction groove, drops into milk of lime, and control pH value 10～11 is fully reacted 20～25min, and underflow contains solid-liquid and removes the sludge concentration basin, goes the band filter press filtration after concentrating;
(d) add the PAM flocculation agent to the secondary neutralization reaction slip that generates, mixed solution is squeezed into the dense precipitation machine of II level highly effective coagulation through pump;
(e) medial launder is gone in top stillness of night overflow, adds anti-clear liquid pH value to 6～9 of transferring of sulfuric acid in medial launder; Underflow contains solid-liquid and removes the sludge concentration basin, goes the band filter press filtration after concentrating;
(f) water outlet is further removed SS and residual fine suspension from the filtering basin that flow into the band grid, and it is multiplexing that last clear water can return phosphoric acid plant, also direct qualified discharge.
Contain phosphoric acid salt and fluorochemical in the phosphorus-containing wastewater, in first step neutralization reaction, add milk of lime, can remove the fluorochemical of most of (about 75%) in the waste water, generate insoluble Calcium Fluoride (Fluorspan), this moment, the pH value was about 5～6, the calcium phosphate that generates solubility simultaneously enters the second stage, and this is very beneficial to second stage defluorination.Calcium phosphate and Calcium Fluoride (Fluorspan) reaction generate the calcium monofluorophosphate (Ca of indissoluble
5(PO
4)
3F).This receiving electrode indissoluble and water are so can remove most of phosphate radical and remaining fluorochemical.After the sedimentation of the second stage, fluorochemical in the supernatant liquor and phosphate concn can be reduced to lower aq, satisfy the requirement of qualified discharge.
Chemical reaction is as follows:
2F-+Ca
2+→CaF
2↓
3HPO
4 2-+5Ca
2++3OH
-+F
-→Ca
5(PO
4)
3F↓+3H
2O；
Fluorine, phosphonium ion molar weight are calculated in sampling earlier before adding milk of lime, calculate calcium ion molar weight, the amount that directly obtains dropping into milk of lime of adding according to above-mentioned reaction formula again.
Phosphorus-containing wastewater adopts the neutralization of secondary lime, the dense depositing technology of secondary highly effective coagulation to handle, and has good dephosphorization, defluorination effect.Phosphorus-containing wastewater is squeezed into I level neutralization reaction pond through pump, add milk of lime, pH value 5～6 in the control flume makes waste water be the milkiness shape, generates the calcium phosphate of Calcium Fluoride (Fluorspan) precipitation and solubility this moment, before pumping into I level highly effective coagulation thickening pond, add flocculation agent, make turbid liquid carry out flocculation reaction in the groove inner central tube, after particle aggregation became greatly, sedimentation was quickened, carry out sufficient mud-water separation, remove the Calcium Fluoride (Fluorspan) precipitation; II level neutralization reaction pond is gone in the water outlet overflow, the same milk of lime that directly adds, and control pH value about 10～11, calcium phosphate in the water and Calcium Fluoride (Fluorspan) reaction generate the calcium monofluorophosphate (Ca of indissoluble
5(PO
4)
3F), remove by II level highly effective coagulation thickening pond.Water outlet is from flowing into medial launder, after adding that sulfuric acid is counter and transferring stillness of night pH value to 6～9.Flow in the filtering basin of band grid and filter, further remove SS and residual fine suspension, water outlet flows into clean water basin, and it is multiplexing to return phosphoric acid plant, also direct qualified discharge.
The filtrate of above-mentioned sludge concentration basin is returned I level neutralization reaction pond and is utilized.
The weight ratio that adds the consumption of milk of lime in the above-mentioned one-level neutralization reaction in the consumption of adding milk of lime and the secondary neutralization reaction is 7: 3.It is best to draw this additional proportion neutralization through overtesting, and does not also waste milk of lime.
The mud of the dense precipitation machine of I and II highly effective coagulation adopts the self-priming sludge pump regularly to handle, after being evacuated to sludge thickener and concentrating by sludge pump, squeeze into the belt filter press processed by pump again, dirty slag main component after the dehydration is calcium phosphate, Calcium Fluoride (Fluorspan), lime carbonate and calcium sulfate, as the phosphate rock resource fully recovering, filtrate flows back to I level neutralization reaction groove.
Beneficial effect: the present invention has realized the multiplexing or qualified discharge of waste water, and the zero release of sludge meets the developing direction of China's energy-saving and emission-reduction, recycling economy.By the phosphorous hydrochlorate of the clear liquid after this art breading (with P
2O
5Meter) 0.4～0.5mg/L, F 8～9mg/L, COD 60～80mg/L satisfy GB8978-1996 primary standard emission request, and it is multiplexing that last clear liquid can return phosphoric acid plant, also direct qualified discharge; The main component of filtering the waste residue that produces is calcium phosphate, Calcium Fluoride (Fluorspan), lime carbonate and calcium sulfate, makes the phosphate rock resource fully recovering.
Description of drawings
Fig. 1 is a process flow sheet of the present invention.
Embodiment
Embodiment 1
(1) the phosphorus-containing wastewater metering is sampled to waste water after pump is squeezed into I level neutralization reaction pond, measures fluorine, phosphonium ion molar weight, calculates the amount that drops into milk of lime again.Add neutralizing agent milk of lime, pH value 5 in the control flume, control air-flow stirring velocity is 5L/min, makes waste water be the milkiness shape, fully reacts 30min; (2) add the PAM flocculation agent to one-level neutralization reaction slip, mixed solution is squeezed into the dense precipitation machine of I level highly effective coagulation through pump; (3) top stillness of night overflow enters II level neutralization reaction groove, drops into neutralizing agent milk of lime, and control pH value 10 is fully reacted 25min, and underflow contains solid-liquid and removes the sludge concentration basin, goes the band filter press filtration after concentrating; (4) add the PAM flocculation agent to the secondary neutralization reaction slip that generates, mixed solution is squeezed into the dense precipitation machine of II level highly effective coagulation through pump; (5) medial launder is gone in top stillness of night overflow, adds the anti-stillness of night pH value to 6 of transferring of sulfuric acid in medial launder; Underflow contains solid-liquid and removes the sludge concentration basin, goes the band filter press filtration after concentrating; (6) water outlet is further removed SS and residual fine suspension from the filtering basin that flow into the band grid, and it is multiplexing that last clear water can return phosphoric acid plant, also direct qualified discharge.
Embodiment 2
(1) the phosphorus-containing wastewater metering is sampled to waste water after pump is squeezed into I level neutralization reaction pond, measures fluorine, phosphonium ion molar weight, calculates the amount that drops into milk of lime again.Add neutralizing agent milk of lime, pH value 6 in the control flume, control air-flow stirring velocity is 5L/min, makes waste water be the milkiness shape, fully reacts 250min; (2) add the PAM flocculation agent to one-level neutralization reaction slip, mixed solution is squeezed into the dense precipitation machine of I level highly effective coagulation through pump; (3) top stillness of night overflow enters II level neutralization reaction groove, drops into neutralizing agent milk of lime in proportion, and control pH value 11 is fully reacted 20min, and underflow contains solid-liquid and removes the sludge concentration basin, goes the band filter press filtration after concentrating; (4) add the PAM flocculation agent to the secondary neutralization reaction slip that generates, mixed solution is squeezed into the dense precipitation machine of II level highly effective coagulation through pump; (5) medial launder is gone in top stillness of night overflow, adds the anti-stillness of night pH value to 9 of transferring of sulfuric acid in medial launder; Underflow contains solid-liquid and removes the sludge concentration basin, goes the band filter press filtration after concentrating; The filtrate of described sludge concentration basin of while is returned I level neutralization reaction pond and is utilized.(6) water outlet is further removed SS and residual fine suspension from the filtering basin that flow into the band grid, and it is multiplexing that last clear water can return phosphoric acid plant, also direct qualified discharge.
Embodiment 3
(1) the phosphorus-containing wastewater metering is sampled to waste water after pump is squeezed into I level neutralization reaction pond, measures fluorine, phosphonium ion molar weight, calculates the amount that drops into milk of lime again.Add neutralizing agent milk of lime earlier, add-on is 70% of a total amount, pH value 6 in the control flume, and control air-flow stirring velocity is 5L/min, makes waste water be the milkiness shape, fully reacts 25min; Fully react 28min; (2) add the PAM flocculation agent to one-level neutralization reaction slip, mixed solution is squeezed into the dense precipitation machine of I level highly effective coagulation through pump; (3) top stillness of night overflow enters II level neutralization reaction groove, adds the neutralizing agent milk of lime of remaining 30% amount again, and control pH value 11 is fully reacted 22min, and underflow contains solid-liquid and removes the sludge concentration basin, goes the band filter press filtration after concentrating; (4) add the PAM flocculation agent to the secondary neutralization reaction slip that generates, mixed solution is squeezed into the dense precipitation machine of II level highly effective coagulation through pump; (5) medial launder is gone in top stillness of night overflow, adds the anti-stillness of night pH value to 8 of transferring of sulfuric acid in medial launder; Underflow contains solid-liquid and removes the sludge concentration basin, goes the band filter press filtration after concentrating; The filtrate of described sludge concentration basin of while is returned I level neutralization reaction pond and is utilized.(6) water outlet is further removed SS and residual fine suspension from the filtering basin that flow into the band grid, and it is multiplexing that last clear water can return phosphoric acid plant, also direct qualified discharge.
Claims (4)
1. the phosphorus-containing wastewater that produces in the multiple fertile production process of a phosphorus and the treatment process of sludge, carry out according to the following steps: pending phosphorus-containing wastewater adds milk of lime earlier, control pH value 5～6 is carried out the neutralization reaction first time, adds the PAM flocculation agent then and carries out mud-water separation after the flocculation reaction; Water adds milk of lime once more, and control pH value 10～11 is carried out the neutralization reaction second time, adds the PAM flocculation agent once more and carries out mud-water separation after the flocculation reaction, and water reaches emission standard after filtering.
2. according to the phosphorus-containing wastewater that produces in the multiple fertile production process of the described phosphorus of claim 1 and the treatment process of sludge, it is characterized in that carrying out as follows:
(a) the phosphorus-containing wastewater metering adds milk of lime after pump is squeezed into I level neutralization reaction pond, pH value 5～6 in the control flume, and control air-flow stirring velocity is 5L/min, makes waste water be the milkiness shape, fully reacts 25～30min;
(b) add the PAM flocculation agent to one-level neutralization reaction slip, mixed solution is squeezed into the dense precipitation machine of I level highly effective coagulation through pump;
(c) the upper clear supernate overflow enters II level neutralization reaction groove, drops into milk of lime, and control pH value 10～11 is fully reacted 20～25min, and underflow contains solid-liquid and removes the sludge concentration basin, goes the band filter press filtration after concentrating;
(d) add the PAM flocculation agent to the secondary neutralization reaction slip that generates, mixed solution is squeezed into the dense precipitation machine of II level highly effective coagulation through pump;
(e) medial launder is gone in top stillness of night overflow, adds anti-clear liquid pH value to 6～9 of transferring of sulfuric acid in medial launder; Underflow contains solid-liquid and removes the sludge concentration basin, goes the band filter press filtration after concentrating;
(f) water outlet is further removed SS and residual fine suspension from the filtering basin that flow into the band grid, and it is multiplexing that last clear water can return phosphoric acid plant, also direct qualified discharge.
3. according to the phosphorus-containing wastewater that produces in the multiple fertile production process of the described phosphorus of claim 2 and the treatment process of sludge, it is characterized in that: the filtrate of described sludge concentration basin is returned I level neutralization reaction pond and is utilized.
4. according to the phosphorus-containing wastewater that produces in claim 2 or the multiple fertile production process of 3 described phosphorus and the treatment process of sludge, it is characterized in that: the weight ratio that adds the consumption of milk of lime in the described one-level neutralization reaction in the consumption of adding milk of lime and the secondary neutralization reaction is 7: 3.
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| CN102381785A (en) * | 2011-10-20 | 2012-03-21 | 瓮福（集团）有限责任公司 | Method for recovering waste water containing phosphorus |
| CN102491472A (en) * | 2011-11-24 | 2012-06-13 | 瓮福（集团）有限责任公司 | Method for recovering sewage slag and preparing phosphate concentrate by using sewage slag |
| CN102503589A (en) * | 2011-10-20 | 2012-06-20 | 瓮福（集团）有限责任公司 | Method for recycling phosphorus-containing wastewater residue from phosphate fertilizer plant |
| CN102616958A (en) * | 2012-03-29 | 2012-08-01 | 安徽省天虹绿洲环保科技有限公司 | Treatment technology of low concentration electroplating wastewater |
| CN102633384A (en) * | 2012-04-20 | 2012-08-15 | 瓮福（集团）有限责任公司 | Method for preparing phosphoric acid by recycling phosphorus from phosphorus-containing wastewater |
| CN102690000A (en) * | 2012-05-11 | 2012-09-26 | 湖北富邦科技股份有限公司 | Method for recovering phosphorus in phosphorus chemical wastewater by using struvite production technology |
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| CN104787935A (en) * | 2015-05-07 | 2015-07-22 | 东北电力大学 | Fluorine-containing wastewater treatment method |
| CN105254073A (en) * | 2015-11-05 | 2016-01-20 | 四川新能水处理工程有限公司 | System and implementation method for treating and recycling wastewater from phosphorus chemical industry |
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| CN102381785A (en) * | 2011-10-20 | 2012-03-21 | 瓮福（集团）有限责任公司 | Method for recovering waste water containing phosphorus |
| CN102503589A (en) * | 2011-10-20 | 2012-06-20 | 瓮福（集团）有限责任公司 | Method for recycling phosphorus-containing wastewater residue from phosphate fertilizer plant |
| CN102491472A (en) * | 2011-11-24 | 2012-06-13 | 瓮福（集团）有限责任公司 | Method for recovering sewage slag and preparing phosphate concentrate by using sewage slag |
| CN102491472B (en) * | 2011-11-24 | 2013-07-17 | 瓮福（集团）有限责任公司 | Method for recovering sewage slag and preparing phosphate concentrate by using sewage slag |
| CN102616958A (en) * | 2012-03-29 | 2012-08-01 | 安徽省天虹绿洲环保科技有限公司 | Treatment technology of low concentration electroplating wastewater |
| CN102633384A (en) * | 2012-04-20 | 2012-08-15 | 瓮福（集团）有限责任公司 | Method for preparing phosphoric acid by recycling phosphorus from phosphorus-containing wastewater |
| CN102690000A (en) * | 2012-05-11 | 2012-09-26 | 湖北富邦科技股份有限公司 | Method for recovering phosphorus in phosphorus chemical wastewater by using struvite production technology |
| CN103073126A (en) * | 2013-01-24 | 2013-05-01 | 中国高岭土有限公司 | Treatment method of kaolin mineral processing waste water |
| CN103539287A (en) * | 2013-10-30 | 2014-01-29 | 江西自立资源再生有限公司 | Sewage treatment system |
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| CN104787935A (en) * | 2015-05-07 | 2015-07-22 | 东北电力大学 | Fluorine-containing wastewater treatment method |
| CN105254073A (en) * | 2015-11-05 | 2016-01-20 | 四川新能水处理工程有限公司 | System and implementation method for treating and recycling wastewater from phosphorus chemical industry |
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| CN109205854A (en) * | 2018-10-29 | 2019-01-15 | 贵州川恒化工股份有限公司 | The new method of the synchronous deep phosphorous removal fluorine of the inorganic sewage of phosphorous chemical industry |
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| CN110498537A (en) * | 2019-09-03 | 2019-11-26 | 瓮福（集团）有限责任公司 | A kind of technique that the phosphorus fluorine sewage containing ammonia nitrogen efficiently removes ammonia nitrogen |
| CN110563198A (en) * | 2019-09-04 | 2019-12-13 | 广西长润环境工程有限公司 | Chemical fertilizer wastewater treatment method and treatment equipment |
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