CN106518174B - The method that a kind of phosphorus in extraction sludge produces phosphorous compound fertilizer - Google Patents
The method that a kind of phosphorus in extraction sludge produces phosphorous compound fertilizer Download PDFInfo
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- CN106518174B CN106518174B CN201610969807.5A CN201610969807A CN106518174B CN 106518174 B CN106518174 B CN 106518174B CN 201610969807 A CN201610969807 A CN 201610969807A CN 106518174 B CN106518174 B CN 106518174B
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- phosphorus
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Classifications
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05B—PHOSPHATIC FERTILISERS
- C05B17/00—Other phosphatic fertilisers, e.g. soft rock phosphates, bone meal
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/37—Phosphates of heavy metals
- C01B25/375—Phosphates of heavy metals of iron
-
- 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
-
- 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
- C02F11/02—Biological treatment
- C02F11/04—Anaerobic treatment; Production of methane by such processes
Abstract
The problems such as present invention proposes a kind of phosphorus method that produces phosphorous compound fertilizer in extraction sludge, and solution releases that phosphorus effect is poor, and energy consumption is high in the prior art, and heavy metal is adulterated in phosphorus regenerant.The method is realized in the following manner: (1) phosphorus discharges: acid solution being added into sludge solutions, discharges into phosphate in solution；(2) phosphorus recycles: taking out phosphatic supernatant is contained in step (1), by the way that Fe is added3+Make PO4 3‑With Fe3+Ferric phosphate precipitating is generated on a preset condition based, and ferric phosphate precipitating is washed several times；(3) prepared by phosphate fertilizer: reducing agent is added into ferric phosphate precipitating, by Fe3+It is reduced into Fe2+, and along with PO4 3‑Dissolution；It adds MgO, Mg (OH)2, CaO or Ca (OH)2PH is adjusted, phosphorous composite fertilizer material is formed, phosphorous composite fertilizer material is processed into phosphorous compound fertilizer.The present invention can turn waste into wealth, and the phosphor resourceization in sludge is utilized, to the resource utilization rate of phosphorus in sludge up to 92% or more.
Description
Technical field
The present invention relates to sludge treatment field, and in particular to a kind of phosphorus extracted in sludge produces the side of phosphorous compound fertilizer
Method.
Background technique
Phosphorus in nature is limited and non-renewable non-metallic mineral resource, is mainly used for agricultural fertilizer, disappears every year
Consumption is very big, and phosphorus ore has been cited as China is not able to satisfy national economic development needs one of 20 kinds of mineral products after 2010.And
During the biochemical treatment of sewage, microorganism can accumulate excessive phosphorus in the form of poly- phosphorus, and in addition there are iron phosphorus, aluminium phosphorus, calcium
The generation of the precipitatings such as phosphorus, so that the content of phosphorus is quite high in sludge, up to the 6.9% of mud dry weight, great recovery value.Cause
This is released the phosphorus in sludge by effective ways, and is recycled with certain forms, not the only processing of sludge
Disposition and resource utilization open a new direction, also reduce the loss of phosphorus and phosphorus loss bring water in nature
Body eutrophication is of great significance to promoting the ensured sustained development of phosphor resource to utilize.
In terms of the recycling of phosphorus, more pay attention to both at home and abroad, but without formation Research foundation.Phosphorus in municipal sludge
Method for releasing mainly include the following types: aerobic/anaerobic digestion method, low energy consumption, it is longer to release the phosphorus period, generally require 15 days with
On；Ozonation dissolves the autoxidation that cytosis strengthens bacterium by ozone, destroys cell membrane, make intracellular matter
It can accelerate ground to be dissolved in liquid phase, the dissolution rate of such method is lower；Heat treating process to release phosphorus effect preferable, but energy consumption is higher；
Acid, alkali soluble born of the same parents' method to release phosphorus effect best.The recovery method of phosphorus has ammoniomagnesium phosphate crystal method, potassium-sodium phosphates magnesium crystallisation, phosphoric acid
Calcium salt class compound precipitation method etc., but inevitably have heavy metal ion doping during releasing phosphorus in the liquid phase, the above phosphorus recycling
Method all can be precipitated together, be crystallized with heavy metal.
Therefore, phosphorus cost-effective cannot be released and safely be recycled by existing method, for example, application number
The method recycled for CN200810106419.X, notification number CN101580334A, entitled sludge phosphorus from urban sewage treatment plant
Patent in, use the mode that combines for 1 ~ 5 with microwave reaction of acidification pH to discharge in sludge in the sludge after gravity concentration
Phosphorus, then phosphorus recycling is carried out using calcium phosphate crystal method control pH=7.8 ~ 11.The method to be heated up using microwave radiation discharges phosphorus
Effect it is limited, and energy consumption is high, and microwave reactor is at high cost；Plurality of heavy metal enters in rich phosphorus liquid in acidization, directly adjusts
PH=7.8 ~ 11 recycling phosphorus are saved, then recycles species and contains plurality of heavy metal, be unfavorable for the resource utilization of product.
Therefore, a kind of phosphorus extracted in sludge efficiently releasing phosphorus technology and combining with the phosphorus recovery technology of economic security is developed
The method for producing phosphorous compound fertilizer is particularly significant.
Summary of the invention
The present invention proposes a kind of method that the phosphorus extracted in sludge produces phosphorous compound fertilizer, solves phosphorus in the prior art and releases
It is poor to put effect, energy consumption is high, in phosphorus regenerant the problems such as doping heavy metal.
The technical scheme of the present invention is realized as follows: a kind of method that the phosphorus extracted in sludge produces phosphorous compound fertilizer,
It realizes in the following manner:
(1) phosphorus discharges: acid solution being added into sludge solutions after mixing, adjusts pH < 4, makes the phosphoric acid in sludge
Salt discharges into solution from solid sludges；
(2) phosphorus recycles: will release the sludge solutions quiescent setting after phosphorus in step (1), will take containing phosphatic supernatant
Out, to containing Fe is added in phosphatic supernatant3+, so that PO4 3-With Fe3+Ferric phosphate precipitating is generated on a preset condition based, and
Ferric phosphate precipitating is washed several times；
(3) prepared by phosphate fertilizer: reducing agent is added into ferric phosphate precipitating, by Fe3+It is reduced into Fe2+, and along with PO4 3-It is molten
Out；Continue to add MgO, Mg (OH)2, CaO or Ca (OH)2Turbid solution adjusts pH, forms phosphorous composite fertilizer material, will be phosphorous compound
Fertile Raw material processing forms phosphorous compound fertilizer.Preferably, step (1) chemistry first carries out Anaerobic Treatment to sludge before releasing phosphorus.
The anaerobic reaction is room temperature anaerobism 3 ~ 7 days or anaeration in normal temperature 1 ~ 3 day.
Reducing agent in the step (3) is hydrogen sulfide gas or sodium sulfide solution or sodium hydrosulfide.
The hydrogen sulfide gas generated during the Anaerobic Treatment process and phosphorus release is as the reduction in step (3)
Agent.
The solid content of sludge solutions after mixing in the step (1) is 3% ~ 10%.
Acid solution in the step (1) is organic acid soln or dilute mineral acid solution.
The preset condition of the step (2) is specifically PO4 3-With Fe3+Molar ratio is 1:1 ~ 1.5, and pH value of solution > 2 are stirred to react
Time > 10min.
PH to 5 ~ 9 is adjusted in the step (3).
Compared with prior art, the invention has the following advantages that
1, the method that the phosphorus of the present invention extracted in sludge produces phosphorous compound fertilizer, using anaerobic reaction and chemistry side
The mode that method combines carries out releasing phosphorus, and low energy consumption, method is simple, reagent cost is low, it is short to release the phosphorus period, and it is good to release phosphorus effect, warp
Cross verifying, the present invention to the resource utilization rate of phosphorus in sludge up to 92% or more, it is economical, effectively, safety by the phosphorus in sludge
Resource utilization；
2, the method that the phosphorus of the present invention extracted in sludge produces phosphorous compound fertilizer is carried out in rich phosphorus liquid using molysite
The recycling of phosphorus can obtain ferric phosphate precipitating under the conditions of lower pH, and be washed several times to ferric phosphate precipitating, effectively anti-
Only in phosphorus removal process heavy metal doping, guarantee the quality of final phosphorous compound fertilizer；
3, the method that the phosphorus of the present invention extracted in sludge produces phosphorous compound fertilizer, discharged in Anaerobic Treatment and phosphorus
Cheng Zhonghui generates hydrogen sulfide gas, and the hydrogen sulfide gas of generation is collected to and is used for the preparation of phosphorous composite fertilizer material, effectively anti-
Stop pollution of the foul smell to environment, while also saving the preparation cost of phosphorous compound fertilizer.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
Some embodiments of invention for those of ordinary skill in the art without creative efforts, can be with
It obtains other drawings based on these drawings.
Fig. 1 is the process flow chart for the method that a kind of phosphorus extracted in sludge of the present invention produces phosphorous compound fertilizer.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, those of ordinary skill in the art are obtained every other under that premise of not paying creative labor
Embodiment shall fall within the protection scope of the present invention.
As shown in Figure 1, a kind of method that the phosphorus extracted in sludge produces phosphorous compound fertilizer is realized in the following manner:
(1) phosphorus discharges: acid solution being added into sludge solutions after mixing, adjusts pH < 4, makes the phosphoric acid in sludge
Salt discharges into solution from solid sludges, this releases phosphorus for chemistry；
(2) phosphorus recycles: the sludge solutions quiescent setting after chemistry to be released to phosphorus will take out containing phosphatic supernatant, to
Containing Fe is added in phosphatic supernatant3+, so that PO4 3-With Fe3+Ferric phosphate precipitating is generated on a preset condition based, and to phosphoric acid
Iron precipitating is washed several times；
(3) prepared by phosphate fertilizer: reducing agent is added into ferric phosphate precipitating, by Fe3+It is reduced into Fe2+, and along with PO4 3-It is molten
Out；Continue to add MgO, Mg (OH)2, CaO or Ca (OH)2Turbid solution adjusts pH, forms phosphorous composite fertilizer material, will be phosphorous compound
Fertile Raw material processing forms phosphorous compound fertilizer.
Preferably, sludge is first carried out Anaerobic Treatment before releasing phosphorus by step (1) chemistry.Under anaerobic state, poly- phosphorus
Bacterium will cause intracellular phosphatic increase, a part of increased phosphoric acid by decomposing poly- phosphorus and part glycogen as energy source
Salt is discharged to extracellularly in such a way that active is spread by corresponding carrier, increases the phosphate concn in sludge solutions.
The anaerobic reaction is room temperature anaerobism 3 ~ 7 days or medium temperature (35 ~ 40 DEG C) anaerobism 1 ~ 3 day.
In the present invention, the reducing agent is hydrogen sulfide gas or sodium sulfide solution or sodium hydrosulfide.
Preferably, anaerobic reaction and chemistry, which release the hydrogen sulfide gas after phosphorus, can be used as reducing agent in step (3).Hydrogen sulfide
It can be used as reducing agent recycling to use, for the preparation of phosphorous compound fertilizer, can both prevent pollution of the foul smell to environment, it can be with
Save the preparation cost of phosphorous compound fertilizer.
The solid content of sludge solutions in the step (1) after mixing is 3% ~ 10%.
Acid solution in the step (1) is organic acid soln or dilute mineral acid solution, the dilute mineral acid solution packet
Dilute sulfuric acid, dilute hydrochloric acid, dust technology, dilute perchloric acid etc. are included but are not limited only to, the organic acid soln includes but are not limited to vinegar
Acid, glacial acetic acid etc..
Wherein, the preset condition of step (2) is specifically PO4 3-With Fe3+Molar ratio is 1:1 ~ 1.5, and pH value of solution > 2, stirring is instead
Between seasonable > 10min.
PH to 5 ~ 9 is adjusted in the step (3).
Working principle of the present invention is as follows: the phosphorus in sludge exists with various forms, including poly- phosphorus, iron phosphorus, aluminium phosphorus, calcium phosphorus
Etc., iron phosphorus, aluminium phosphorus, the calcium phosphorus etc. in sludge are dissolved in such a way that chemistry releases phosphorus, phosphate is shifted from solid sludges
The poly- phosphorus in excess sludge is first decomposed by soluble phosphoric acid by Anaerobic Treatment into sludge solutions, or before chemistry releases phosphorus
Salt releases phosphorus efficiency to improve.
Contain a large amount of heavy metal in sludge, part heavy metal certainly will be released together during releasing phosphorus, if
Extract the heavy metal being doped with during phosphorus in sludge in sludge, it will the quality for influencing phosphate fertilizer pollutes the environment, because
The extraction process of this phosphate fertilizer need to carry out strict control to parameter.The phosphate such as iron phosphorus, aluminium phosphorus, calcium phosphorus are in neutral conditions with phosphoric acid
Salt precipitation form exists, and the pH of conditioning of mud solution dissolves whole phosphate in sludge.
The reaction equation of citric acid soluble phosphorus (calcium magnesium phosphate, phosphoric acid phosphate fertilizer and steel slag phosphorus etc.) preparation is as follows:
6FePO4+3Na2S→2Fe3(PO4)2+3S+6Na++2PO4 3-
Fe3(PO4)2+4CaO→Ca4P2O9+3FeO
Fe3(PO4)2+4Ca(OH)2→Ca4P2O9+3FeO+4H2O
Compared with prior art, the present invention obtains that phosphorous compound fertilizer is non-hygroscopic, does not agglomerate, is not soluble in water, is dissolved in neutral lemon
Lemon acid ammonium solution, according to GBT 22549-2008 standard detection, citric acid soluble phosphorus content in the phosphorous compound fertilizer that is prepared in the present invention
Greater than 20%.
Embodiment 1:
The present embodiment carries out as steps described below:
The excess sludge of certain sewage treatment plant is adjusted into solid content 5%, is uniformly mixed sludge solutions；To after mixing
Sludge in be added dilution heat of sulfuric acid, adjust pH=2, phosphate enters in solution from solid sludges after reacting 1h；After reaction
Sludge solutions quiescent setting will take out containing phosphatic supernatant, and measure the PO in solution4 3-Concentration is 579mg/L；Xiang Han
Have in phosphatic solution and Fe is added3+, so that PO4 3-With Fe3+Molar ratio be 1:1, be added CaO turbid solution adjust pH value of solution=
3, canescence ferric phosphate FePO is generated after reacting 10min4Precipitating；Sodium hydrosulfide is added into ferric phosphate precipitating, by Fe3+Also
Original is at Fe2+, and along with PO4 3-Dissolution；Continue to add CaO turbid solution adjusting pH=7 after reaction 1h, is formed and precipitate processed obtains
Phosphate fertilizer.
Embodiment 2:
The present embodiment carries out as steps described below:
Certain secondary sedimentation tank of sewage treatment work sludge room temperature anaerobism 3 days, conditioning of mud solid content 10% are uniformly mixed；It is molten to sludge
Dilute hydrochloric acid solution is added in liquid, adjusts pH=0.5, phosphate enters in solution from solid sludges after reacting 30min, and sludge is molten
Liquid quiescent setting will take out containing phosphatic supernatant, and measure the PO in solution4 3-Concentration is 513mg/L；To containing phosphoric acid
A certain amount of Fe is added in the solution of salt3+, so that PO4 3-With Fe3+Molar ratio be 1:1.5, adjust pH value of solution=2.5, reaction
Canescence ferric phosphate FePO is generated after 15min4Precipitating；Hydrogen sulfide gas is passed through into ferric phosphate precipitating, reaction is after a certain period of time
Continue to add CaO turbid solution adjusting pH=7.5 or so, forms precipitating processing and obtains phosphate fertilizer.
Embodiment 3:
The present embodiment carries out as steps described below:
Certain sludge of sewage treatment plant room temperature anaerobism 7 days adjusts 3% or more solid content, is uniformly mixed sludge solutions；To mixed
Glacial acetic acid solution is added in sludge after closing uniformly, adjusts pH=2, phosphate enters solution from solid sludges after reacting 40min
In, sludge solutions quiescent setting will take out containing phosphatic supernatant, and measure the PO in solution4 3-Concentration is 799mg/L；To
Containing a certain amount of Fe is added in phosphatic solution3+, so that PO4 3-With Fe3+Molar ratio be 1:1.2, adjust pH value of solution=4,
Canescence ferric phosphate FePO is generated after reacting 12min4Precipitating；Sodium hydrosulfide is added into ferric phosphate precipitating, reaction is certain
Continue to add Ca (OH) after time2Turbid solution adjusts pH=8, and formation precipitating is processed to obtain phosphate fertilizer.
Embodiment 4:
The present embodiment carries out as steps described below:
Certain sludge of sewage treatment plant anaeration in normal temperature 1 day 40 DEG C of temperature, adjusts solid content 7% or more, to after mixing
Acetum is added in sludge, adjusts pH=1.5, phosphate enters in solution from solid sludges after reaction 1.5 hours, sludge
Solution stand precipitating will be taken out containing phosphatic supernatant, and measure the PO in solution4 3-Concentration is 56mg/L；To containing phosphoric acid
A certain amount of Fe is added in the solution of salt3+, so that PO4 3-With Fe3+Molar ratio be 1:1, adjust pH value of solution=2.2, reaction
Canescence ferric phosphate FePO is generated after 40min4Precipitating；Sodium sulfide solution is added into ferric phosphate precipitating, reaction is after a certain period of time
Continue to add Ca (OH)2Turbid solution adjusts pH=6, and formation precipitating is processed to obtain phosphate fertilizer.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Within mind and principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (1)
1. a kind of method that the phosphorus extracted in sludge produces phosphorous compound fertilizer, it is characterised in that: to sludge room temperature Anaerobic Treatment 7
It, the solid content of conditioning of mud solution is 3% or more, is uniformly mixed sludge solutions；Ice is added into sludge after mixing
Acetic acid solution, so that sludge solutions pH=2, react 40min, phosphate enters in solution from solid sludges, and sludge solutions are static
Precipitating will be taken out containing phosphatic supernatant, and measure the PO in solution4 3-Concentration is 799mg/L；To containing phosphatic molten
A certain amount of Fe is added in liquid3+, so that PO4 3-With Fe3+Molar ratio be 1:1.2, adjust pH value of solution=4, react 12min, generate
Canescence ferric phosphate FePO4Precipitating；Sodium hydrosulfide is added into ferric phosphate precipitating, reaction continues to add Ca after a certain period of time
(OH)2Turbid solution, so that pH value of solution=8, the precipitating of formation is processed to obtain phosphorous compound fertilizer.
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Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107540182A (en) * | 2017-10-20 | 2018-01-05 | 天津壹新环保工程有限公司 | A kind of method and apparatus of sludge organic fertilizer |
| CN109081536B (en) * | 2018-08-28 | 2021-08-24 | 合肥市市政设计研究总院有限公司 | Method for recovering anaerobic ammonium oxidation sludge from chemical sludge |
| CN110540479B (en) * | 2019-09-19 | 2022-05-31 | 东北农业大学 | Sludge recycling treatment method |
| CN112938917B (en) * | 2021-01-28 | 2022-11-04 | 北京大学 | Preparation method of efficient nano-phosphate fertilizer and nano-phosphate fertilizer |
| CN113401887B (en) * | 2021-07-12 | 2022-07-19 | 湖北云翔聚能新能源科技有限公司 | Method for preparing iron phosphate by using municipal sludge incineration ash and battery-grade iron phosphate |
| CN113772905B (en) * | 2021-09-22 | 2022-09-09 | 同济大学 | Method for directionally and cleanly recovering phosphorus in sludge through alkali heat treatment |
| CN115367974B (en) * | 2022-07-25 | 2024-04-16 | 浙江大学 | Device and method for recycling phosphorus-containing muddy water based on magnetic adsorbent |
| CN116924378B (en) * | 2023-09-18 | 2023-12-12 | 内蒙古大学 | Method for directionally cleaning and recycling phosphorus in sludge through acid-regulated hydrothermal carbonization reforming treatment |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104609688A (en) * | 2015-01-04 | 2015-05-13 | 同济大学 | Method for improving phosphorus release rate of iron phosphate-containing sludge during anaerobic fermentation |
| CN106007292A (en) * | 2016-07-15 | 2016-10-12 | 天津壹新环保工程有限公司 | Method and device for respectively extracting and using inorganic matters in sludge |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104609688A (en) * | 2015-01-04 | 2015-05-13 | 同济大学 | Method for improving phosphorus release rate of iron phosphate-containing sludge during anaerobic fermentation |
| CN106007292A (en) * | 2016-07-15 | 2016-10-12 | 天津壹新环保工程有限公司 | Method and device for respectively extracting and using inorganic matters in sludge |
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