CN108689585A - A method of recycling phosphorus from cryogenic freezing and microwave combined pretreating sludge supernatant - Google Patents
A method of recycling phosphorus from cryogenic freezing and microwave combined pretreating sludge supernatant Download PDFInfo
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- CN108689585A CN108689585A CN201810517177.7A CN201810517177A CN108689585A CN 108689585 A CN108689585 A CN 108689585A CN 201810517177 A CN201810517177 A CN 201810517177A CN 108689585 A CN108689585 A CN 108689585A
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F11/00—Treatment of sludge; Devices therefor
- C02F11/18—Treatment of sludge; Devices therefor by thermal conditioning
- C02F11/20—Treatment of sludge; Devices therefor by thermal conditioning by freezing
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F11/00—Treatment of sludge; Devices therefor
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/105—Phosphorus compounds
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Abstract
A method of it recycling phosphorus from cryogenic freezing and microwave combined pretreating sludge supernatant, belongs to city sewage and sludge processing technology field.It is discharged into the situation in supernatant for phosphate difficulty in excess sludge, this method uses cryogenic freezing and microwave combined pretreated mode, the phosphate concn in excess sludge is greatly improved.When excess sludge freezes 23h under the conditions of -20 DEG C, then the sludge solutions pH value after cryoablation is adjusted to 4 with the hydrochloric acid of a concentration of 3mol/L, it is 700W to be put into power, elder generation microwave 30s and then stop 30s with this standing wave 5min repeatedly in the micro-wave oven that frequency is 2450MHz, phosphate maximum concentration can reach 280 ± 50mg/L, the supernatant that finally centrifugation is obtained is 9.5, Mg in pH:P molar ratios are 1.8, and agitation revolution reacts 20min under conditions of being 200r/min, and precipitation 50min can greatly improve the efficiency of phosphorus recycling.It is of the invention economical, simple, reliable.
Description
Technical field
The invention belongs to water pollution controls and resource regeneration field, are related to a kind of from cryogenic freezing and microwave combined pre-
Handle the method that phosphorus is recycled in sludge supernatant.
Background technology
Phosphorus is nutrient needed for important all organisms, it plays and can not replace in agricultural and industrial development
The important function in generation.The economic development and population increase of rapid advances make the demand of P chemical fertilizer and chemical products be stepped up.Example
Such as, Tilman et al. predicts that the demand of phosphate fertilizer will be from 3.43 × 10 in 20007Ton increases to the 4.76 × 10 of the year two thousand twenty7Ton,
The year two thousand fifty is up to 8.37 × 107Ton.On the other hand, mineral P is the limited non-renewable resources of reserves.Its quick consumption figure
Nature supply is all being reduced rapidly every year.It is estimated that if not taking intervening measure, global phosphoric acid salt reserve will be in 100 years
Interior exhaustion.Therefore, in order to realize the sustainable development of phosphor resource, recycling phosphate is of great significance from waste.
Sewage is largely flowed by the phosphor resource that mankind's exploitation utilizes and enters sewage treatment plant, and in sewage disposal process
In, phosphorus is finally trapped in excess sludge again, and the excess sludge of the nutrients such as rich Nitrogen-and Phosphorus-containing can be referred to as " to misplace position
Resource ", for this purpose, recycle phosphorus from sludge, on the one hand reduce phosphorus and enter the risk that water body generates eutrophication, on the other hand
It is the important conception excavated the second phosphorus ore and solve world's phosphor resource shortage problem.Therefore, a large amount of phosphorus are recycled from liquid phase sludge
Technical research is most important.It has developed several for recycling phosphatic technology from the liquid phase of sludge.Wherein most base
In calcium phosphate precipitation or crystallization process.However, before recycling phosphate, it is necessary to by phosphate from being discharged into primary sludge
In clear liquid, then precipitated with calcium phosphate or ammonium magnesium phosphate (MAP or guanite).Recently, developed various biologies, physics and
Chemical method, such as acid and basic hydrolysis, wet oxidation, ultrasound hydrolysis, chlorine dioxide treatment and microwave radiation are opened
Send decomposition sludge.Some available methods either need addition chemical substance to come initiation reaction or the reaction of longer time.
Cryogenic freezing processing makes dirt as a kind of effective sludge conditioning means it is verified that can improve the dewatering of sludge
Mud grain structure is even closer, reduces and combines water content, can also realize sludge disintegration simultaneously, and subsequent phosphate is accelerated to discharge
Process.Compared with Mechanical Method needs a large amount of energy consumptions and chemical method to need to add chemical agent, the refrigerating process of cryogenic freezing processing
It spontaneous can carry out and (be particularly suitable for cold district or winter climate), it is simple for process, number of polymers, operation need not be used
Expense can substantially reduce.The phosphate in sludge is discharged using microwave radiation, because it has heats speed than conventional heating techniques
The advantages that rate higher, computer heating control is more preferable, equipment size and smaller waste.Therefore, for seek rapidly and efficiently phosphorus release
Process using the phosphate in cryogenic freezing and microwave combined preconditioning technique release sludge, and is studied by chemical precipitation
Phosphatic organic efficiency in clear liquid, minimizing and recycling to realize sludge recycle.
The present invention is technically different from using phosphorus is recycled from cryogenic freezing and microwave combined pretreating sludge supernatant
The prior art is mainly reflected in following two aspect:
(1) during this investigation it turned out, the solution of the activated sludge of sewage treatment plant is pre-processed by cryogenic freezing.In order to
Phosphatic release in sludge, pretreated sludge solutions is further promoted to radiate under microwave condition.It is tried by single factor test
It tests and has inquired into cooling time, microwave sludge solutions pH value, the influence that the microwave time discharges phosphate in sludge.
(2) phosphate discharged in cryogenic freezing and microwave radiation process integration pretreating sludge is utilized, it is heavy by chemistry
It forms sediment and studies phosphatic organic efficiency in supernatant.Sludge solutions pH value, Mg have been inquired by single factor experiment:P molar ratios,
Speed of agitator, the influence that the reaction time recycles phosphate in sludge.
Invention content
Present invention aims at provide a kind of utilize in cryogenic freezing and microwave combined pretreatment reinforcement sludge supernatant times
The method for receiving phosphorus.This method is short reaction time, at low cost, while can increase the biodegradability of excess sludge and phosphatic production
Amount improves the phosphate rate of recovery, realizes minimizing and the recycling of sludge, with good economic efficiency.
Technical scheme of the present invention:
(1) it is derived from the excess sludges of MUCT technique secondary settling tanks precipitation concentration 12h at room temperature;
(2) remove the supernatant after concentration, the sludge suspension solid concentration SS after precipitation concentration is 16000 ± 1000mg/
L;
(3) 23h is freezed under the conditions of the sludge after precipitation concentration being placed in -20 DEG C;
(4) sludge after freezing is melted completely at room temperature, after adding the hydrochloric acid of a concentration of 3mol/L to adjust freezing
Sludge solutions pH value to 4;
(5) it is 700W the sludge solutions after adjustment pH to be put into power, and frequency is first microwave in the micro-wave oven of 2450MHz
Then 30s stops 30s with this standing wave 5min repeatedly;
(6) sludge solutions after microwave are remained with 5000r/min centrifugations 5min by 0.45 μm of membrane filtration at this time
Phosphate concn in remaining sludge supernatant reaches 280 ± 50mg/L;
(7) it is 9.5, Mg in pH by the supernatant for centrifuging film acquisition:P molar ratios are 1.8, agitation revolution 200r/min
Under conditions of, 20min is reacted, precipitation 50min is to realize that phosphorus recycles.
The present invention has the advantage that compared with prior art:
The present invention provides a kind of side recycling phosphorus using cryogenic freezing and in microwave combined pretreatment reinforcement sludge supernatant
Method belongs to city sewage and sludge processing technology field.Phosphate is recycled from the liquid phase of sludge, wherein most is based on phosphate
Precipitation or crystallization process.However, phosphorus concentration is relatively low in sludge condensation supernatant, undigested sludge liquor, it is often small
In 100mg/L, therefore before recycling phosphate, it is necessary to phosphate is discharged into from primary sludge in supernatant, then with
Calcium phosphate or ammonium magnesium phosphate (MAP or guanite) precipitation.It is discharged into the situation in supernatant for phosphate difficulty in excess sludge,
This method uses cryogenic freezing and microwave combined pretreated mode, and the phosphate concn in excess sludge is greatly improved.From
And improve the efficiency of phosphate recycling.Not only solve the problem that the phosphate rate of recovery is low under low concentration, and this pre- place
Reason method does not need a large amount of energy consumptions and addition chemical agent, and simple for process, cost-effective and place preferably realizes sludge
Minimizing and recycling.
The innovative point of the present invention:
The present invention utilizes phosphatic release in cryogenic freezing and microwave combined pretreatment reinforcement sludge supernatant, relative to
Common anaerobic fermentation, microwave lysis, cryogenic freezing change sludge by cryogenic freezing first with microwave combined pretreatment
Dewatering keeps sludge structure even closer, realizes that cell cracks, then accelerates cell by microwave radiation and crack to promote
The sludge supernatant containing high concentration phosphorus hydrochlorate is produced in phosphatic release, for studying phosphorus recycling.Phosphorous recovery is set to reach
97% or more.
Description of the drawings
The influence that cooling times different Fig. 1 discharges sludge intracellular phosphate
The influence that the microwave time different Fig. 2 discharges sludge intracellular phosphate
The influence that different sludge solutions pH discharges sludge intracellular phosphate when Fig. 3 microwaves
The influence that pH different Fig. 4 recycles phosphate in sludge supernatant
Mg different Fig. 5:The influence that P molar ratios recycle phosphate in sludge supernatant
The influence that mixings time different Fig. 6 recycles phosphate in sludge supernatant
The influence that speeds of agitator different Fig. 7 recycles phosphate in sludge supernatant
Specific implementation mode
With reference to specific embodiment, the present invention will be further described:
Embodiment 1:
It is derived from the excess sludge precipitation at room temperature concentration 12h of MUCT technique secondary settling tanks;Remove supernatant, the dirt after precipitation concentration
Mud suspended sediment concentration SS is 16300mg/L, pH 6.8.20 are attached separately to after excess sludge after concentration is stirred evenly
1-72h is freezed under the conditions of being placed in -20 DEG C in the centrifuge tube of 50ml.Respectively freezing 1h, 2h, 3h, 5h, 10h, 23h, 34h, 47h,
This 10 time points of 72h take out two centrifuge tubes, melt at room temperature, the 100ml sludge melted completely is added to the burning of 250ml
In cup, the hydrochloric acid of a concentration of 3mol/L is added to adjust the sludge solutions pH value after ablation to 4.Solution after adjustment pH is put into micro-
In wave stove then elder generation microwave 30s stops 30s with this standing wave 5min repeatedly, by the sludge solutions after microwave with 5000r/min from
Heart 5min, by 0.45 μm of membrane filtration, in spectrophotometric measurement at this time excess sludge supernatant phosphate and ammonia nitrogen it is dense
Degree, as shown in Figure 1, phosphate concn reaches highest 280.2mg/L when cooling time is 23h, ammonia nitrogen concentration also reaches highest
For 14.7mg/L.
Embodiment 2:
It is derived from the excess sludge precipitation at room temperature concentration 12h of MUCT technique secondary settling tanks;Remove supernatant, the dirt after precipitation concentration
Mud suspended sediment concentration SS is 16500mg/L, pH 6.7.Excess sludge after concentration is placed in -20 in the plastic bottle of 2L
23h is freezed under the conditions of DEG C, is melted at room temperature after taking out plastic bottle, will respectively be taken 100ml after the sludge uniform stirring melted completely
Be separately added into the beaker of 10 250ml, add the hydrochloric acid of a concentration of 3mol/L adjust the sludge solutions pH after ablation be respectively 2,
3,4,5,6,7,8,9,10,11 this 10 different values will adjust the solution after pH and be put into micro-wave oven first microwave 30s then
Stopping 30s, standing wave 5min passes through 0.45 μm by the sludge solutions after microwave with 5000r/min centrifugation 5min repeatedly with this
Membrane filtration, with the spectrophotometric measurement phosphate and ammonia nitrogen concentration in excess sludge supernatant at this time, as shown in Fig. 2, molten
Phosphate concn reaches highest 230mg/L when liquid pH is 4, and ammonia nitrogen concentration is also up to 50mg/L.
Embodiment 3:
It is derived from the excess sludge precipitation at room temperature concentration 12h of MUCT technique secondary settling tanks;Remove supernatant, the dirt after precipitation concentration
Mud suspended sediment concentration SS is 16200mg/L, pH 6.8.Excess sludge after concentration is placed in -20 in the plastic bottle of 2L
23h is freezed under the conditions of DEG C, is melted at room temperature after taking out plastic bottle, will respectively be taken 100ml after the sludge uniform stirring melted completely
It is separately added into the beaker of 7 250ml, it is 4 to add the hydrochloric acid conditioning of mud solution ph of a concentration of 3mol/L, solution is put into micro-
In wave stove respectively with first microwave 30s then stop 30s with this repeatedly standing wave 1min, 2min, 3min, 4min, 5min, 6min,
7min measures the sludge solutions after microwave with 5000r/min centrifugations 5min by 0.45 μm of membrane filtration with spectrophotometric
Phosphate and ammonia nitrogen concentration in excess sludge supernatant at this time, as shown in figure 3, phosphate concn reaches most in microwave 5min
High 285mg/L, ammonia nitrogen concentration are also up to 26.4mg/L.
Embodiment 4:
It is derived from the excess sludge precipitation at room temperature concentration 12h of MUCT technique secondary settling tanks;Remove supernatant, the dirt after precipitation concentration
Mud suspended sediment concentration SS is 17000mg/L, pH 6.8.Excess sludge after concentration is placed in -20 in the plastic bottle of 2L
23h is freezed under the conditions of DEG C, melts 3h at room temperature after taking out plastic bottle, it will be after the sludge uniform stirring melted completely plus a concentration of
The hydrochloric acid conditioning of mud solution ph of 3mol/L is 4, then solution, which is put into micro-wave oven elder generation microwave 30s, stops 30s with this repeatedly
Sludge solutions after microwave are centrifuged 5min, by 0.45 μm of membrane filtration, with light splitting by standing wave 5min with 5000r/min
Luminosity measures the phosphate and ammonia nitrogen concentration in excess sludge supernatant at this time, respectively takes 100ml to be separately added into 6 supernatant
In the conical flask of 150ml, with Mg:P molar ratios are 1.6 magnesium ion solutions that a concentration of 1mol/L is added, and add a concentration of 2mol/L
Sodium hydroxide solution adjust solution pH value be respectively 8,8.5,9,9.5,10,10.5, be put into six blenders with 200r/
Min stirs 20min, precipitates 50min, measures phosphate and ammonia nitrogen concentration in surplus solution supernatant with spectrophotometric later,
Remaining mole and the their own removal rate of phosphate and ammonia nitrogen are calculated as shown in figure 4, reaching highest when pH is 9.5
The rate of recovery 97.65%.
Embodiment 5:
Supernatant after taking example 3 to centrifuge film measures phosphate and ammonia nitrogen concentration at this time with spectrophotometric, by supernatant
Liquid respectively takes 100ml to be separately added into the conical flask of 6 150ml, with Mg:P molar ratios are respectively 1.2,1.4,1.6,1.8,2,2.2
The magnesium ion solution of a concentration of 1mol/L is added, it is 9.5 to add the sodium hydroxide solution of a concentration of 2mol/L to adjust solution ph, is put
Enter in six blenders and 20min is stirred with 200r/min, precipitate 50min, measures surplus solution supernatant with spectrophotometric later
In phosphate and ammonia nitrogen concentration, calculate remaining mole and the their own removal rate of phosphate and ammonia nitrogen as shown in figure 5,
In Mg:P molar ratios reach the highest rate of recovery 97.4% when being 1.8.
Embodiment 6:
Supernatant after taking example 3 to centrifuge film measures phosphate and ammonia nitrogen concentration at this time with spectrophotometric, by supernatant
Liquid respectively takes 100ml to be separately added into the conical flask of 6 150ml, with Mg:P molar ratios be 1.8 be added the magnesium of a concentration of 1mol/L from
Sub- solution, add a concentration of 2mol/L sodium hydroxide solution adjust solution pH value be 9.5, be put into six blenders with
200r/min stirs 10min, 20min, 30min, 40min, 50min, 60min respectively, precipitates 50min, uses spectrophotometric later
The phosphate and ammonia nitrogen concentration in surplus solution supernatant are measured, the remaining mole and each of phosphate and ammonia nitrogen are calculated
Removal rate as shown in fig. 6, mixing time be 20min when reach the highest rate of recovery 97.4%.
Embodiment 7:
Supernatant after taking example 3 to centrifuge film measures phosphate and ammonia nitrogen concentration at this time with spectrophotometric, by supernatant
Liquid respectively takes 100ml to be separately added into the conical flask of 6 150ml, with Mg:P molar ratios are 1.8 magnesium ions that concentration 1mol/L is added
Solution, add a concentration of 2mol/L sodium hydroxide solution adjust solution pH value be 9.5, be put into six blenders respectively with
150r/min, 200r/min, 300r/min, 400r/min, 500r/min, 600r/min stir 20min, precipitate 50min, later
The phosphate and ammonia nitrogen concentration in surplus solution supernatant are measured with spectrophotometric, calculates the remaining mole of phosphate and ammonia nitrogen
With their own removal rate as shown in fig. 7, reaching the highest rate of recovery 98.4% when rotating speed is 200r/min.
Claims (2)
1. a kind of method recycling phosphorus from cryogenic freezing and microwave combined pretreating sludge supernatant, which is characterized in that including
Following steps:
(1) it is derived from the excess sludges of MUCT technique secondary settling tanks precipitation concentration 12h at room temperature;
(2) remove the supernatant after concentration, the sludge suspension solid concentration SS after precipitation concentration is 16000 ± 1000mg/L;
(3) 23h is freezed under the conditions of the sludge after precipitation concentration being placed in -20 DEG C;
(4) sludge after freezing is melted completely at room temperature, the sludge solutions pH value after adjustment freezing to 4;
(5) it is 700W the sludge solutions after adjustment pH to be put into power, and frequency is first microwave 30s in the micro-wave oven of 2450MHz
Then stop 30s with this standing wave 5min repeatedly;
(6) sludge solutions after microwave are centrifuged into 5min with 5000r/min, it is remaining at this time dirty by 0.45 μm of membrane filtration
Phosphate concn in mud supernatant reaches 280 ± 50mg/L;
(7) it is 9.5, Mg in pH by the supernatant for centrifuging film acquisition:P molar ratios are 1.8, and agitation revolution is the item of 200r/min
Under part, 20min is reacted, precipitation 50min is to realize that phosphorus recycles.
2. according to the method described in claim 1, it is characterized in that:It is adjusted using the hydrochloric acid of a concentration of 3mol/L in step (4)
Sludge solutions pH value after freezing is to 4.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114394725A (en) * | 2022-01-17 | 2022-04-26 | 同济大学 | Method for improving anaerobic digestion of sludge to produce methane by combination of freezing and calcium hypochlorite |
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| GB1459175A (en) * | 1972-10-17 | 1976-12-22 | Atomic Energy Authority Uk | Treatment of sludges |
| CN1377324A (en) * | 1999-08-10 | 2002-10-30 | 格伦·斯普林斯控股公司 | Recovery of element phosphorus from phosphorus sludge |
| CN101695999A (en) * | 2009-10-23 | 2010-04-21 | 宁波工程学院 | Method for recovering nutritive materials of phosphorus and nitrogen from sewage and sludge |
| CN103043838A (en) * | 2012-12-26 | 2013-04-17 | 大连春兴科技股份有限公司 | Freezing and thawing treatment method for suspended wastewater |
| CN206266403U (en) * | 2016-10-18 | 2017-06-20 | 中节能博实(湖北)环境工程技术股份有限公司 | One kind freezing and ultrasonic combined deep dehydration processing system |
| CN106904807A (en) * | 2017-03-31 | 2017-06-30 | 同济大学 | A kind of method that phosphorus is reclaimed from dewatered sludge |
-
2018
- 2018-05-25 CN CN201810517177.7A patent/CN108689585B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1459175A (en) * | 1972-10-17 | 1976-12-22 | Atomic Energy Authority Uk | Treatment of sludges |
| CN1377324A (en) * | 1999-08-10 | 2002-10-30 | 格伦·斯普林斯控股公司 | Recovery of element phosphorus from phosphorus sludge |
| CN101695999A (en) * | 2009-10-23 | 2010-04-21 | 宁波工程学院 | Method for recovering nutritive materials of phosphorus and nitrogen from sewage and sludge |
| CN103043838A (en) * | 2012-12-26 | 2013-04-17 | 大连春兴科技股份有限公司 | Freezing and thawing treatment method for suspended wastewater |
| CN206266403U (en) * | 2016-10-18 | 2017-06-20 | 中节能博实(湖北)环境工程技术股份有限公司 | One kind freezing and ultrasonic combined deep dehydration processing system |
| CN106904807A (en) * | 2017-03-31 | 2017-06-30 | 同济大学 | A kind of method that phosphorus is reclaimed from dewatered sludge |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114394725A (en) * | 2022-01-17 | 2022-04-26 | 同济大学 | Method for improving anaerobic digestion of sludge to produce methane by combination of freezing and calcium hypochlorite |
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