CN103641283A - Method of economically recycling phosphor from excess sludge - Google Patents
Method of economically recycling phosphor from excess sludge Download PDFInfo
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- CN103641283A CN103641283A CN201310610599.6A CN201310610599A CN103641283A CN 103641283 A CN103641283 A CN 103641283A CN 201310610599 A CN201310610599 A CN 201310610599A CN 103641283 A CN103641283 A CN 103641283A
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Abstract
The invention relates to a method of economically recycling phosphor from excess sludge. The method comprises the following steps: (1), pre-treating the excess sludge; (2), carrying out alkaline hydrolysis on the excess sludge, wherein the alkaline hydrolysis is carried out by a single-stage alkaline hydrolysis method or a two-stage alkaline hydrolysis method; measuring concentration of orthophosphate and ammonia nitrogen in liquid supernatant; and (3), adding magnesium salt aqueous liquor with a Mg/P molar ratio of 0.8-2, stirring and reacting for 10 minutes-120 minutes, gravitationally or centrifugally separating precipitates, naturally drying the precipitates to obtain a magnesium ammonium phosphate crude product. Organic substances remained in the liquid supernatant can be used for producing methane by anaerobic fermentation or supplementing a carbon source by a reflux wastewater treatment system, also can be used for supplementing alkalinity needed for an anaerobic unit, so that comprehensive utilization of excess sludge is facilitated. The method disclosed by the invention has the advantages that nutrient elements in the sludge are comprehensively utilized, process is simple, and phosphor can be recycled by only adding the magnesium salt; and meanwhile, ammonia nitrogen can be partly recycled without regulating pH, and the obtained magnesium ammonium phosphate crude product can be used for producing fertilizers.
Description
Technical field
The present invention relates to a kind of sludge treatment and dispose and resource utilization method, belong to water treatment field.Be specifically related to a kind of method that reclaims phosphorus from excess sludge of economy.
Background technology
Along with the quickening of China's Development of China's Urbanization, urban wastewater discharge constantly increases, and the mud that sewage work produces the particularly amount of excess sludge is increasing.Expectation to 2015 year, municipal sludge amount will reach 759.4 ten thousand tons, and this numerical value also can continue to increase within for some time.General sludge treatment disposal costs accounts for the more than 50% of sewage work's overall running cost, needs huge fund input.Meanwhile, mud is also a kind of available resource, contains the nutritive elements such as the needed nitrogen of plant-growth, phosphorus, potassium and maintains the various trace elements that plant normal growth grows and organism and the soil ulmin that can improve Soil structure.Therefore, if can realize the recycling of mud, can alleviate to a certain extent the operation working expense of sewage work, also be conducive to environment protection.
Phosphorus is the source of all things on earth growing nutrient, but is a kind of very limited and non-renewable natural Mineral resources.In municipal effluent, contain a large amount of phosphorus, enter excess sludge and be removed in sewage treatment process, therefore, the potentiality that reclaim phosphorus from excess sludge are very large.From mud, reclaim phosphorus, not only useful and Sustainable development, can also create considerable economic benefit.Facts have proved, it is feasible by chemical method, carrying out phosphorus recovery.Use now more chemical recovering method phosphorus conventionally to have magnesium ammonium phosphate (MgNH
4pO
46H
2o, MAP, is commonly called as struvite) precipitator method and calcium phosphate salt (the being HAP) precipitator method.Due to magnesium ammonium phosphate method recyclable part ammonia nitrogen when reclaiming phosphorus, and magnesium ammonium phosphate is good slow release fertilizer, so be considered to the most promising phosphorus, reclaims approach.In theory, as long as contain magnesium ion, ammonia nitrogen and ortho-phosphoric acid in solution, the long-pending solubility product constant that is greater than magnesium ammonium phosphate of their ionic concn, and pH is at 8.5-10.0 alkaline range, just has magnesium ammonium phosphate and generates.
Because the phosphorus in mud had both been present in extracellular polymeric, be present in again in born of the same parents, therefore first must make it to be discharged in supernatant liquor by preprocessing means redeposition separation and recycling.Reported that the pretreating sludges such as acid system, By Ozone, supersonic method, microwave method and heating method discharge the research of phosphorus.But they are except the facility investment of self with power consumption medicine expends, also there is an extra-pay: the supernatant liquor obtaining due to these processing modes is slant acidity or closely neutral all, do not reach the desired alkaline range of magnesium ammonium phosphate method, so need to add alkali, regulate pH, and increased reagent cost, more limited the large-scale application of these technology.Adopt alkaline hydrolysis mud to discharge the mode of phosphorus, not only to equipment and energy consumption require lowly, and can save and add the extra-expense that alkali regulates pH, not only economy but also effective.
Summary of the invention
The present invention will solve the expensive problem that reclaims phosphorus from excess sludge, a kind of economical and effective is provided and is conducive to the method that reclaims phosphorus from excess sludge that excess sludge fully utilizes.
For reaching above object, solution of the present invention is:
The method that reclaims phosphorus from excess sludge of a kind of economy that the present invention proposes, its concrete steps are:
(1) excess sludge pre-treatment: excess sludge is passed through to gravity concentration or is diluted to concentration is 10-40 g/L, is equivalent to water ratio 96%-99%, obtains pretreated excess sludge;
(2) excess sludge alkaline hydrolysis: promote the release of phosphorus nitrogen element in excess sludge by single-stage alkaline hydrolysis method or secondary alkaline hydrolysis method, the concentration of orthophosphoric acid salt and ammonia nitrogen in mensuration supernatant liquor, testing method is ammonium molybdate spectrophotometry and nessler reagent spectrophotometry.
(3) in the supernatant liquor that contains ammonia nitrogen and orthophosphoric acid salt obtaining to step (2), add Mg/P mol ratio at the magnesium salt solution of 0.8-2, stirring reaction 10-120min, make the orthophosphoric acid salt and ammonia nitrogen and the magnesium ion formation magnesium ammonium phosphate sediment that in supernatant liquor, contain, gravity or centrifugation throw out, recovery part ammonia nitrogen when reclaiming phosphorus, throw out, through seasoning, obtains magnesium ammonium phosphate crude product.
In aforesaid method, the described single-stage alkaline hydrolysis of step (2) method is specially: the pretreated excess sludge of getting X volume, adding alkali adjusting pH is 10.0-13.0, and stirring reaction 0.5-8h, releases outside born of the same parents the phosphorus nitrogen element of mud, the pretreated excess sludge of 0.5-3.5X volume reinjects, continue stirring reaction 0.5-1h, make pH be down to 8.5-10.0, then at 2000-6000 rpm, carry out centrifugal solid-liquid separation, collect supernatant liquor, be the supernatant liquor that contains ammonia nitrogen and orthophosphoric acid salt.
In aforesaid method, the described secondary alkaline hydrolysis of step (2) method is specially: in first step alkaline hydrolysis reactor, inject the pretreated excess sludge of X volume, in 50-350rpm, stir, alkaline hydrolysis reaction 0.5-8h, make pH regulator to centrifugal discharge supernatant liquor after 8.5-10.0, i.e. first step alkaline hydrolysis water outlet, discharge system; Residual solid after centrifugal, first step alkaline hydrolysis is residual solid, injects second stage alkaline hydrolysis reactor, in the alkaline hydrolysis reactor of the second stage, inject the water of 2/7-5/7X volume, the sodium hydroxide solution with 1-20M when 50-350rpm stirs regulates pH 10.0-13.0, continues alkaline hydrolysis reaction 0.5-8h, the rear centrifugal supernatant liquor that obtains, be secondary alkaline hydrolysis supernatant liquor, inject the reactor of first step alkaline hydrolysis, residual solid after centrifugal, be that secondary alkaline hydrolysis is residual solid, removal system; Recirculation, operation continuously, wherein the water outlet of first step alkaline hydrolysis is the supernatant liquor that contains ammonia nitrogen and orthophosphoric acid salt, and pH is 8.5-10.0.
In aforesaid method, must regulate pH to 8.5-10.0 by step (2), could start to carry out step (3).
In aforesaid method, the described excess sludge concentration of step (1) is controlled at 10-40 g/L and discharges to obtain phosphorus largely.
In aforesaid method, the residual active sludge that described excess sludge is municipal sewage plant, concentration basin mud, dewatered sludge and anaerobically digested sludge, comprise treated excess sludge; Described processing comprises more than one in acid, ultrasonic, heat and ozone.
In aforesaid method, in described alkaline hydrolysis, the form that adds of alkali comprises solid and solution, and wherein strength of solution is at 1-20M, and the kind of alkali comprises sodium hydroxide, potassium hydroxide or calcium hydroxide.
In aforesaid method, described in contain ammonia nitrogen and orthophosphoric acid salt supernatant liquor in orthophosphoric acid salt concentration reach 30-180 mg/L, ammonia nitrogen concentration reaches 20-150 mg/L.
In aforesaid method, described magnesium salt solution comprises magnesium chloride brine, magnesium sulfate solution or the magnesiumcarbonate aqueous solution, or replaces described magnesium salt solution with seawater.
In aforesaid method, the ammonia nitrogen of the recyclable 15%-50% of the method and the orthophosphoric acid salt of 50%-95%, can make TSS and VSS decrement 20%-60% and 30%-80%, and SCOD reaches 2000-10000 mg/L.
In aforesaid method, after separated magnesium ammonium phosphate sediment thing, organism residual in supernatant liquor produces methane or return-flow system supplementary carbon source for anaerobically fermenting, can supplement the basicity that anaerobic unit needs simultaneously, is conducive to the comprehensive utilization of excess sludge.
Know-why of the present invention is: under alkaline condition, hydroxide ion reacts with the acidic-group that maintains the outer polymer architecture of extracellular microbial, promotes protein, polysaccharide, ammonia nitrogen and orthophosphoric acid salt stripping in excess sludge extracellular polymeric; Meanwhile, hydroxide ion can destroy phospholipid bilayer on cytolemma, causes the release of thing (protein, polysaccharide, ammonia nitrogen and orthophosphoric acid salt) in microorganism cells cracking and born of the same parents.Supernatant liquor contains ammonia nitrogen and orthophosphoric acid salt, and pH meets magnesium ammonium phosphate sediment condition, and only needing to add magnesium salts provides appropriate magnesium ion, makes their the long-pending solubility product constant that is greater than magnesium ammonium phosphate of ionic concn, will spontaneous generation magnesium ammonium phosphate sediment thing.
Compared with prior art, positively effect of the present invention is:
(1) the present invention adopts alkaline hydrolysis pre-treatment excess sludge, can make the total phosphorus of about 40%-90% in mud be released in supernatant liquor.Wherein 60%-90% is orthophosphoric acid salt, and corresponding concentration is 30-180 mg/L, is conducive to chemical recovering method phosphorus; In this process, also discharge a certain amount of ammonia nitrogen, its concentration in supernatant liquor is 20-150 mg/L.Meanwhile, supernatant liquor pH is in 8.5-10.0 scope.These conditions can meet the requirement of magnesium ammonium phosphate sediment completely, only need to add magnesium salt solution, can spontaneous a large amount of generation magnesium ammonium phosphate sediments.
(2) the present invention adopts alkaline hydrolysis pre-treatment excess sludge, with (90 ℃ of acid system (38% hydrochloric acid) and heating methods, 2h) pretreating sludge promotes the test-results comparison that phosphorus discharges, and finds that the release ratio of the orthophosphoric acid salt in supernatant liquor that three kinds of methods obtain is all about 2:3.5:1.The successful that acid system and alkaline process promote phosphorus to discharge is better than heating method; Although the effect of alkaline process is not as good as acid system, reagent consumption, far below the latter, has certain superiority while considering.
(3) the present invention is under the optimized operation condition of magnesium ammonium phosphate method, the total phosphorus of 25%-50% and the orthophosphoric acid salt of 50%-95% in the water outlet of recyclable alkaline hydrolysis mud.Part ammonia nitrogen in water outlet simultaneously is also recycled utilization.
(4) the present invention adopts alkaline hydrolysis pre-treatment excess sludge, discharges a large amount of organism, makes the SCOD of supernatant liquor reach 2000-10000 mg/L.After separated magnesium ammonium phosphate sediment thing, organism residual in supernatant liquor both can be back to protista treatment system supplementary carbon source, can produce methane by anaerobically fermenting again, can supplement the basicity that anaerobic unit needs simultaneously, was conducive to the comprehensive utilization of excess sludge.
(5) the present invention adopts alkaline hydrolysis pre-treatment excess sludge, has certain decrement effect, and excess sludge TSS, VSS reduce 20%-60% and 30%-80%, have realized stabilization and the minimizing of mud, are conducive to follow-up sludge disposal.
accompanying drawing explanation:
Fig. 1 is secondary alkaline hydrolysis process flow sheet.
Fig. 2 is the effect that in embodiment 1, in single-stage alkaline hydrolysis process, the lower phosphorus nitrogen of different pH values discharges.
Fig. 3 is the effect that the magnesium ammonium phosphate method in embodiment 2 reclaims phosphorus nitrogen in water outlet.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail:
(1) single-stage alkaline hydrolysis operating process: be the excess sludge of 20 g/L to the concentration of injecting X volume in 6 reactors respectively, the sodium hydroxide solution of 10 M of take when 150 rpm stir regulates and adds alkali to regulate pH be 8.0,9.0,10.0,11.0,12.0,12.5,13.0,13.5, stirring reaction 1h, the phosphorus nitrogen element of mud is released outside born of the same parents, and this is alkaline hydrolysis mud.As seen from Figure 2, within the scope of pH 10.0-13.5, along with pH raises, more phosphorus nitrogen element is released in the liquid phase of mud, effect highly significant; But after considering pH 13.0, the required amount of sodium hydroxide adding sharply increases, and the more suitable pH condition of choosing is 13.0.
(2), in alkaline hydrolysis mud, the concentration of injecting X volume in the reactor that is directly 13.0 in step (1) pH condition is that the excess sludge of 20 g/L mixes, and continues stirring reaction 1h, makes pH be down to 9.6.Then at 4000 rpm, carry out centrifugal solid-liquid separation, collect supernatant liquor, record the concentration of orthophosphoric acid salt and ammonia nitrogen in supernatant liquor and be respectively 70 mg/L and 65.5 mg/L.Now, centrifugal rear residual solid TSS and VSS reduce by 40% and 55% than excess sludge, have reached stabilization effect, are conducive to subsequent disposal and dispose.
(3) according to the volumetric molar concentration of the orthophosphoric acid salt in supernatant liquor and content, add wherein Mg/P mol ratio and be 1.4 magnesium salts, 100 rpm stirring reaction 10min are to occurring a large amount of precipitations, gravity or centrifugation throw out, seasoning, obtains magnesium ammonium phosphate crude product.Meanwhile, the organic concentration of centrifugal rear supernatant liquor is high, and SCOD is 2570 mg/L, is applicable to do carbon source or anaerobically fermenting and produces methane;
(4) this process characteristic is: simple to operate, equipment investment and running cost are low.
(1) secondary alkaline hydrolysis operating process as shown in Figure 1, in first step alkaline hydrolysis reactor A, is injected the pretreated excess sludge 1 of X volume, and its concentration is 20 g/L, is equivalent to water ratio 98%, in 150rpm, stirs, and alkaline hydrolysis reaction 1h, makes pH regulator to 9.2-9.4.Then centrifugal discharge supernatant liquor, i.e. first step alkaline hydrolysis water outlet 6, discharge system; Residual solid after centrifugal, first step alkaline hydrolysis is residual solid 2, injects second stage alkaline hydrolysis reactor.In the alkaline hydrolysis reactor B of the second stage, inject the water of 3/7X volume, the sodium hydroxide solution with 10M when 150rpm stirs regulates pH13.0, continues alkaline hydrolysis reaction 1h.Then the centrifugal supernatant liquor that obtains, i.e. secondary alkaline hydrolysis supernatant liquor 5, injects the reactor of first step alkaline hydrolysis; Residual solid after centrifugal, secondary alkaline hydrolysis is residual solid 3, removal system.Recirculation, continuously operation.In whole operating process, what finally discharge system is residual solid (sludge stream is to being designated solid line), and the water adding and alkali are finally discharged system (supernatant liquor flows to and is designated dotted line) with water outlet.Wherein, after residual solid 3 dehydrations, TSS and VSS have reduced 30%-40% and 40%-50% than excess sludge, have reached stabilization effect, and directly sanitary landfill is processed; First step alkaline hydrolysis water outlet 6 is the supernatant liquor that contains ammonia nitrogen (62.5-64.5 mg/L) and orthophosphoric acid salt (62-64 mg/L), and pH is 9.2-9.4.
(2) measure the concentration of the orthophosphoric acid salt in water outlet 6, according to its volumetric molar concentration amount, add wherein respectively the magnesium salts of 0,1.0,1.4,1.6,1.8 and 2.0 times of mole number, 100 rpm stirring reaction 10min are to occurring a large amount of precipitations, gravity or centrifugation throw out, seasoning, obtains magnesium ammonium phosphate crude product.As seen from Figure 3, the magnesium salts amount adding is at 0-1.4 times in the scope of orthophosphoric acid salt volumetric molar concentration, and along with throwing the rising of magnesium amount, the phosphorus nitrogen element in water outlet is more reclaimed, and generates magnesium ammonium phosphate product; But the rate of recovery of phosphoric (orthophosphoric acid salt) remains unchanged after 1.4 times, no longer include magnesium ammonium phosphate and produce, therefore the more suitable throwing magnesium amount (Mg/P ratio) of choosing is 1.4.Meanwhile, organic concentration high (SCOD is 2330-2360 mg/L) in centrifugal rear supernatant liquor, is applicable to do carbon source or anaerobically fermenting and produces methane.
(3) feature of this technique is: with respect to embodiment 1, can reduce alkali and consume 15%-50%.
The above-mentioned description to embodiment is can understand and apply the invention for ease of those skilled in the art.Person skilled in the art obviously can easily make various modifications to these embodiment, and General Principle described herein is applied in other embodiment and needn't passes through performing creative labour.Therefore, the invention is not restricted to the embodiment here, those skilled in the art are according to announcement of the present invention, and the improvement of making for the present invention and modification all should be within protection scope of the present invention.
Claims (9)
1. an economic method that reclaims phosphorus from excess sludge, is characterized in that, its method is as follows:
(1) excess sludge pre-treatment: excess sludge is passed through to gravity concentration or is diluted to concentration is 10-40 g/L, is equivalent to water ratio 96%-99%, obtains pretreated excess sludge;
(2) excess sludge alkaline hydrolysis: promote the release of phosphorus nitrogen element in excess sludge by single-stage alkaline hydrolysis method or secondary alkaline hydrolysis method, the concentration of orthophosphoric acid salt and ammonia nitrogen in mensuration supernatant liquor;
(3) in the supernatant liquor that contains ammonia nitrogen and orthophosphoric acid salt obtaining to step (2), add Mg/P mol ratio at the magnesium salt solution of 0.8-2, stirring reaction 10-120min, make the orthophosphoric acid salt and ammonia nitrogen and the magnesium ion formation magnesium ammonium phosphate sediment that in supernatant liquor, contain, gravity or centrifugation throw out, recovery part ammonia nitrogen when reclaiming phosphorus, throw out, through seasoning, obtains magnesium ammonium phosphate crude product.
2. the method that reclaims phosphorus from excess sludge of a kind of economy as claimed in claim 1, it is characterized in that, the described single-stage alkaline hydrolysis of step (2) method is specially: the pretreated excess sludge of getting X volume, adding alkali adjusting pH is 10.0-13.0, stirring reaction 0.5-8h, the phosphorus nitrogen element of mud is released outside born of the same parents, the pretreated excess sludge of 0.5-3.5X volume reinjects, continue stirring reaction 0.5-1h, make pH be down to 8.5-10.0, then at 2000-6000 rpm, carry out centrifugal solid-liquid separation, collect supernatant liquor, be the supernatant liquor that contains ammonia nitrogen and orthophosphoric acid salt.
3. the method that reclaims phosphorus from excess sludge of a kind of economy as claimed in claim 1, it is characterized in that, the described secondary alkaline hydrolysis of step (2) method is specially: in first step alkaline hydrolysis reactor, inject the pretreated excess sludge of X volume, in 50-350rpm, stir, alkaline hydrolysis reaction 0.5-8h, makes pH regulator to centrifugal discharge supernatant liquor after 8.5-10.0, be the water outlet of first step alkaline hydrolysis, discharge system; Residual solid after centrifugal, first step alkaline hydrolysis is residual solid, injects second stage alkaline hydrolysis reactor, in the alkaline hydrolysis reactor of the second stage, inject the water of 2/7-5/7X volume, the sodium hydroxide solution with 1-20M when 50-350rpm stirs regulates pH 10.0-13.0, continues alkaline hydrolysis reaction 0.5-8h, the rear centrifugal supernatant liquor that obtains, be secondary alkaline hydrolysis supernatant liquor, inject the reactor of first step alkaline hydrolysis, residual solid after centrifugal, be that secondary alkaline hydrolysis is residual solid, removal system; Recirculation, operation continuously, wherein the water outlet of first step alkaline hydrolysis is the supernatant liquor that contains ammonia nitrogen and orthophosphoric acid salt, and pH is 8.5-10.0.
4. the method that reclaims phosphorus from excess sludge of a kind of economy as claimed in claim 1, it is characterized in that, described excess sludge is residual active sludge, concentration basin mud, dewatered sludge and the anaerobically digested sludge of municipal sewage plant, comprises treated excess sludge; Described processing comprises more than one in acid, ultrasonic, heat and ozone.
5. the method that reclaims phosphorus from excess sludge of a kind of economy as claimed in claim 1, it is characterized in that, in described alkaline hydrolysis, the form that adds of alkali comprises solid and solution, and wherein strength of solution is at 1-20M, and the kind of alkali comprises sodium hydroxide, potassium hydroxide or calcium hydroxide.
6. the method that reclaims phosphorus from excess sludge of a kind of economy as claimed in claim 1, is characterized in that, described in contain ammonia nitrogen and orthophosphoric acid salt supernatant liquor in orthophosphoric acid salt concentration reach 30-180 mg/L, ammonia nitrogen concentration reaches 20-150 mg/L.
7. the method that reclaims phosphorus from excess sludge of a kind of economy as claimed in claim 1, is characterized in that, described magnesium salt solution comprises magnesium chloride brine, magnesium sulfate solution or the magnesiumcarbonate aqueous solution, or replaces described magnesium salt solution with seawater.
8. the method that reclaims phosphorus from excess sludge of a kind of economy as claimed in claim 1, it is characterized in that, the method reclaims the ammonia nitrogen of 15%-50% and the orthophosphoric acid salt of 50%-95%, makes TSS and VSS decrement 20%-60% and 30%-80%, and makes supernatant liquor SCOD reach 2000-10000 mg/L.
9. the method that reclaims phosphorus from excess sludge of a kind of economy as claimed in claim 1, it is characterized in that, after separated magnesium ammonium phosphate sediment thing, organism residual in supernatant liquor produces methane or return-flow system supplementary carbon source for anaerobically fermenting, supplement the basicity that anaerobic unit needs simultaneously, be conducive to the comprehensive utilization of excess sludge.
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