CN105772484B - A kind of recovery method of municipal sludge incineration residue innoxious process for treating and phosphorus compound - Google Patents
A kind of recovery method of municipal sludge incineration residue innoxious process for treating and phosphorus compound Download PDFInfo
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- CN105772484B CN105772484B CN201610168605.0A CN201610168605A CN105772484B CN 105772484 B CN105772484 B CN 105772484B CN 201610168605 A CN201610168605 A CN 201610168605A CN 105772484 B CN105772484 B CN 105772484B
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- filtrate
- residue
- sludge
- phosphate
- phosphorus
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09B—DISPOSAL OF SOLID WASTE
- B09B3/00—Destroying solid waste or transforming solid waste into something useful or harmless
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09B—DISPOSAL OF SOLID WASTE
- B09B3/00—Destroying solid waste or transforming solid waste into something useful or harmless
- B09B3/10—Destroying solid waste or transforming solid waste into something useful or harmless involving an adsorption step
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09B—DISPOSAL OF SOLID WASTE
- B09B5/00—Operations not covered by a single other subclass or by a single other group in this subclass
Abstract
The invention discloses a kind of municipal sludge incineration residue harmless treatment and the recovery method of phosphorus compound, step to be：A. rich phosphorus excess sludge is obtained from bioanalysis dephosphorization city domestic sewage system, excess sludge is burned so that while sludge calorific value is utilized, phosphorus is deposited in sludge incineration ash in the form of phosphate；B. carry out soda acid joint to the incineration residue in a to leach so that P elements are discharged into supernatant in the form of positive phosphorus acid ion；C. by magnesium ammonium phosphate sediment method, ammoniomagnesium phosphate crystal thing is obtained；D. the sludge lime-ash after the dissolution of soda acid joint is handled rich phosphorus waste water as adsorbent, repeats b, c process.Raw material is easy to get, easy to implement the method, easy to operate, and this method while heavy metals removal, can will obtain rich phosphorus solution and be reclaimed to obtain high-quality phosphate fertilizer with ammoniomagnesium phosphate crystal method in municipal sludge incineration residue.
Description
Technical field
The invention belongs to environmental technology field, and in particular to municipal sludge incineration residue innoxious process for treating and phosphorus
The recovery of compound, it is applied to the innoxious of municipal sludge incineration residue, phosphorous mine tailing etc., recycling and chemistry
Phosphorus reclaims and the recovery of leachate phosphorus.
Background technology
Phosphorus is one of indispensable nutrient in vital movement, and it plays irreplaceable in the vital movement of cell
Effect.In biosphere, the major part of phosphorus is one-way flow, without Efficient Cycle.Phosphate resource is also thus as one kind
Unrenewable resource, standing crop is fewer and fewer, and phosphorus ore is largely exploited in particular with industrial expansion and accelerates this damage
Lose.For phosphorus during environment (including rock, soil and water), biology and human circulation is participated in, it turns into again simultaneously causes ring
A kind of important component of border pollution.Popularization with Sewage Biological Treatment and the raising to specific resistance to filtration requirement, it is remaining dirty
Mud sustained production is high.Based on being disposed to excess sludge processing, burning turns into proper disposal options.In sludge incineration ash
Phosphorus（With P2O5Meter）Content can reach 8%, be a kind of potential phosphor resource.But the presence of heavy metal is to it in sludge burning ash residue
Use range has made strict limitation, therefore by sludge burning ash residue heavy metals removal and therefrom recovery phosphorus establishes artificial phosphorus
Circulation, it has also become sludge burning ash residue harmless treatment and the important directions for solving phosphorus crisis.
Along with the leaching of heavy metal while sludge burning ash residue phosphorus leaches.Municipal sludge burning ash acid leaching liquor
The heavy metals such as middle Ge, Zn, Cu, Pb partly or entirely easily exceed agricultural standards, have thereby resulted in recovery product agrochemical direction
Application.The highest content of each heavy metal species is defined in agriculture phosphate fertilizer standard, therefore removes removing heavy metals so that product reaches agriculture
It is to have to solve the problems, such as with standard.The country there is no correlation using Ore Leaching alkali precipitation recovery municipal sludge incineration residue
The report of middle phosphorus.
Compared to traditional calcium phosphate phosphate fertilizer, ammonium magnesium phosphate is a kind of high-quality sustained release phosphatization fertilizer.Under near-neutral sulfite deinking, phosphoric acid
Ammonium magnesium has relatively low solubility without causing burn seedlings, and fertility hold period is longer, and will not shine into the hardening soil, is agricultural phosphate fertilizer
Optimal selection.
The content of the invention
The purpose of the present invention is to be the provision of a kind of municipal sludge incineration residue harmless treatment and phosphorus compound
Recovery method, raw material is easy to get, easy to implement the method, easy to operate, and this method can be by heavy metal in municipal sludge incineration residue
While removal, obtain rich phosphorus solution and reclaimed to obtain high-quality phosphate fertilizer with ammoniomagnesium phosphate crystal method.
In order to realize above-mentioned purpose, the present invention uses following technical measures：
A kind of municipal sludge incineration residue harmless treatment and the recovery method of phosphorus compound, its step are：
A, sludge anhydration burning：Rich phosphorus excess sludge is obtained from biological phosphate-eliminating city domestic sewage processing system.To richness
Phosphorus excess sludge carries out desiccation, and temperature is kept for 60-100 DEG C, 1-5h so that dewatered sludge moisture content is maintained at less than 40%.Pass through again
The aerobic burning of 900-1000 DEG C of high temperature is crossed to burning, obtains sludge burning ash residue so that organophosphor is converted into Phos and deposited
In incineration residue.
B, soda acid joint dissolution：First acid treatment b：To sludge burning ash residue acid treatment, by adding sulfuric acid, keep solid
Liquor ratio（Solid-to-liquid ratio represents the ratio between incineration residue weight g and the volume ml of acid solution for dissolving herein, similarly hereinafter）1：4 to 1：10 it
Between, pH is between 0.4-0.6 or so, 15-35 DEG C of temperature for regulation, mixing speed 50-200r/min, mixing time 1-2h, filtering
Obtain the first filtrate III and the first residue IV；Second alkali process c：Alkali process is carried out to the first residue IV, keeps pH=11-13, Gu
Liquor ratio 1：4 to 1：10, between 15-35 DEG C of temperature, mixing speed 50-200r/min, mixing time 1-2h, it is residual to be filtrated to get second
The filtrate VI of slag V and second.
, removal of impurities and recovery：Second filtrate VI is gradually added in the first filtrate III, and stops adding simultaneously in pH=3.0-3.5
Filtering, filtering obtain the 3rd residue VIII and the 3rd filtrate Ⅸ.This measure can be by the iron ion in the first filtrate III, aluminium ion with phosphoric acid
Iron, the form precipitation of aluminum phosphate are the 3rd residue VIII, and the effect of adsorption-edulcoration are played to the fine suspension in solution.By
Two filtrates VI and the 3rd filtrate Ⅸ are according to 3:1 volume ratio is mutually mixed, and adjusts pH of mixed to 9.0- with industrial caustic soda afterwards
11.0, the 4th residue Ⅹ and the 4th filtrate Ⅺ are then filtrated to get, wherein the 4th residue Ⅹ can be used as metallurgical industry raw material.4th
0.5-3.5mol/L magnesium sulfate, 0.5-5.3mol/L ammonium sulfate is added in filtrate Ⅺ；Control magnesium phosphorus mol ratio 1.5-2.0:
1, nitrogen phosphorus mol ratio 2-4:1,15-25min is stood, is filtrated to get the 5th filtrateWith ammoniomagnesium phosphate crystal Ⅻ, the 5th filtrate
It may participate in pH regulation.
, sorbing material attribute testing：Second residue V is carried out 600-650 DEG C, 1-2h calcinings, using solid-liquid（Solid, liquid
The weight g of burning ash and the sour volume ml for dissolving are represented respectively）Than 1：10 pairs of absorbances are 1（It is molten to refer to that light passes through
Incident intensity before liquid or a certain material and the light by the transmitted intensity ratio after solution or material are bottom with 10
Logarithm, be used for characterizing the colourity of waste water from dyestuff herein）Reactive gaudy red X 3B dye waste water carry out adsorption bleaching, mixing speed
50-200r/min, 1-2h, pH=1-10, percent of decolourization is more than 88%.
, product component analysis：XRD test analysis, the purity of ammonium magnesium phosphate crystal Ⅻ can reach 97.0%, wherein about 2%
Magnesium phosphate and magnesium hydroxide, 1% is the mixed phosphate of heavy metal.ICP tests product heavy metal ion as shown by data：In product
Various heavy metal ion can reach agricultural phosphate fertilizer standard, can be used as agriculture slow-release phosphate fertilizer.
Excess sludge of the described rich phosphorus excess sludge after city sewage plant biochemical treatment.
The present invention compared with prior art, has the advantages of following obvious prominent：
（1）Using sludge incineration ash as starting point, with respect to specific resistance to filtration, reduce storage area, avoid because of microorganism
The harmful effect of production environment caused by fermentation.
（2）Phosphorus content is higher compared to rich phosphorous sludge, sewage in sludge incineration ash, organic efficiency can reach 97% be higher than after
Person.
（3）Ammonium magnesium phosphate is agricultural optimal selection as high-quality sustained release agricultural phosphate fertilizer.
（4）Incineration residue after phosphorus extraction, absorption property is excellent, has good treatment effect to colored dyes waste water.
（5）Caused accessory substance can be applied industrially, and soda acid dosage is less.
（6）The present invention is applicable not only to the extraction recovery of sludge incineration ash, while is also applied for phosphorous mine tailing and part
The waste residue of phosphorus ore industry.
Test data shows：A kind of municipal sludge incineration residue harmless treatment and the recovery side of a variety of phosphorus compounds
Method, 87.93% can be reached to the leaching rate of sludge burning ash residue phosphorus, the rate of recovery for leaching phosphorus in rich phosphorus solution can be reached
97.71%, the purity of ammonium magnesium phosphate can reach 97% in crystallized product.
Brief description of the drawings
Fig. 1 is a kind of flow of the recovery method of municipal sludge incineration residue harmless treatment and a variety of phosphorus compounds
Figure.
Embodiment
Embodiment 1：
A kind of municipal sludge incineration residue harmless treatment and the recovery method of a variety of phosphorus compounds, its step are：
1st, rich phosphorus excess sludge I：Experiment is derived from the city domestic sewage of Wuhan City Jiangxia paper mill with rich phosphorus excess sludge
Reason center, it is dirty to sample duration 10h, sampling interval 1h/ times, single sampling amount 200g, average moisture content 79.8%, including setting pot
Mud, digested sludge and excess sludge etc..
2nd, sludge anhydration burning（a）：Desiccation temperature is kept for 100 or 103 or 105 or 108 or 110 DEG C, 3 or 4 or 5h so that
Sludge is dried to constant weight after desiccation；Dewatered sludge is taken to obtain sludge incineration ash through 900 DEG C of 1 or 1.2 or 1.4 or 1.5h of aerobic burning
Slag II, burn and lime-ash phosphorous 4.98% is measured using ammonium molybdate colorimetric method after clearing up.
3rd, acid treatment is filtered（b）：Take and burn the sample 100g of incineration residue II through sulfuric acid solution, solid-to-liquid ratio 1:5, sulfuric acid
Concentration 1-3mol/L, with regulation pH to 0.4 or 0.5 or 0.6, rotating speed 50-200rpm, 20 DEG C of normal temperature processing 1.5 or 1.8 or 2 or
2.2 or 2.4-2.5h, it is filtrated to get the first filtrate III and the first residue IV.
4th, alkali process filters（c）：Alkali process, pH=12.3 or 12.4 or 13.5, solid-to-liquid ratio 1 are carried out to the first residue IV：4-
6, rotating speed 50-200rpm, 15 or 18 or 22 or 26 or 28 or 30 DEG C of Temperature Treatments 1.5 or 1.7 or 1.9 or 2.1 or 2.3 or
2.5h, obtain the second residue V and the second filtrate VI.
5th, calcine（d）：Second residue V is calcined into 1 or 2h at 600 or 610 or 620 or 630 or 640 or 650 DEG C, obtained
Sorbing material VII.
6th, pH=3 or 3.3 or 3.5 filterings are adjusted in ratio mixing（e）：Second filtrate VI is gradually added in filtrate III, and in pH
Filtering obtains residue VIII and filtrate Ⅸ when=3.0 or 3.2 or 3.5.
7th, ratio mixing is adjusted pH=10 or 11 and filtered（f）：Second filtrate VI is completely added in the 4th filtrate Ⅸ, used
Sodium hydroxide adjusts pH=10 or 11, and filtering obtains the 4th filtrate Ⅺ and the 4th residue Ⅹ.
8th, add magnesium source nitrogen source and filter（g）：In pH=10 or 11, magnesium source uses magnesium sulfate, and nitrogen source uses ammonium sulfate, magnesium
Phosphorus ratio is 1.8-2:1, N/P ratio 2-3:Ammoniomagnesium phosphate crystal method precipitation is carried out to the 4th filtrate Ⅺ under the conditions of 1, reacts duration 10
Or 14 or 16 or 18 or 20min, mixing speed 1-200rpm, filter and produce the filtrate Ⅺ of ammonium magnesium phosphate crystal Ⅻ and the 4th.
9th, ratio mixes and adds alkali to filter（h）：By the 5th filtrateIt is added to the second filtrate VI and the 3rd filtrate Ⅸ
In mixed liquor, to reduce the input amount of alkali.
10th, the performance test of sorbing material VII：Test shows：Using solid-to-liquid ratio 1：10（Admittedly refer to sorbing material weight g, liquid
Refer to waste water from dyestuff volume ml）It is 1 to absorbance（Represent the colourity of waste water from dyestuff）Reactive gaudy red X 3B dye waste water carry out
Adsorption bleaching, mixing speed 50-200r/min, 1 or 2h, pH=1 or 3 or 6 or 8 or 10, percent of decolourization more than 88%.
11st, the component analysis of the 3rd residue VIII：Through analyze and process residue VIII be aluminum phosphate and ferric phosphate mixed precipitation, can
Coagulant as pharmaceuticals industry or as sewage disposal.
12nd, the component analysis of the 4th residue Ⅹ：Hydroxide and heavy metal of 4th residue Ⅹ through analysis mainly heavy metal
Phosphate can carry out heavy metal recovery, extract different target metal simple-substance or metallic compound.
13rd, the component analysis of ammonium magnesium phosphate crystal Ⅻ：XRD test analysis, the purity of ammonium magnesium phosphate crystal Ⅻ can reach
97.0%, wherein about 2% magnesium phosphate and magnesium hydroxide, 1% is the mixed phosphate of heavy metal.ICP tests product heavy metal ion
As shown by data, various heavy metal ion can reach agricultural phosphate fertilizer standard in product, can be used as agriculture slow-release phosphate fertilizer.
Excess sludge of the described rich phosphorus excess sludge after city sewage plant biochemical treatment.
The above-mentioned description to implementation process is understood and applied the invention for convenience of those skilled in the art.
One skilled in the art can be modified to example, and the General Principle wherein illustrated is applied in other examples
Without the permission by patent owner.The invention is not restricted to the example implemented here, those skilled in the art are according to this hair
Bright announcement, do not depart from improvement made by scope of the invention and modification all should the present invention scope of patent protection it
Row.
Claims (1)
1. a kind of municipal sludge incineration residue harmless treatment and the recovery method of phosphorus compound, its step are：
A, sludge anhydration burning：Rich phosphorus excess sludge is obtained from biological phosphate-eliminating city domestic sewage processing system, rich phosphorus is remained
Remaining sludge carries out desiccation, and temperature is kept for 60-100 DEG C, 1-5h so that dewatered sludge moisture content is below 40%, then by 900-
The aerobic burning of 1000 DEG C of high temperature obtains sludge burning ash residue, organophosphor is converted into Phos and be deposited on burning ash to burning
In slag；
B, soda acid joint dissolution：First acid treatment（b）：To sludge burning ash residue acid treatment, by adding sulfuric acid, solid-to-liquid ratio is kept
1：4 to 1：Between 10, pH is between 0.4-0.6,15-35 DEG C of temperature for regulation, mixing speed 50-200r/min, mixing time 1-
2h, it is filtrated to get the first filtrate and the first residue（Ⅳ）；Second alkali process（c）：To the first residue（Ⅳ）Alkali process is carried out, is kept
PH=11-13, solid-to-liquid ratio 1：4 to 1：10, between 15-35 DEG C of temperature, mixing speed 50-200r/min, mixing time 1-2h, mistake
Filter obtains the second residue（Ⅴ）With the second filtrate（Ⅵ）；
C, removal of impurities and recovery：Second filtrate（Ⅵ）It is gradually added the first filtrate（Ⅲ）In, and filtered in pH=3.0-3.5, mistake
Filter obtains the 3rd residue（Ⅷ）With the 3rd filtrate（Ⅸ）, by the iron ion in the first filtrate, aluminium ion with ferric phosphate, aluminum phosphate
Form is deposited in the 3rd residue（Ⅷ）, while the effect of adsorption-edulcoration is played to the fine suspension in solution, by the second filtrate
（Ⅵ）With the 3rd filtrate（Ⅸ）According to 3：1 volume ratio is mutually mixed, and adjusts pH of mixed to 9.0-11.0 with industrial caustic soda afterwards,
Then it is filtrated to get the 4th residue（Ⅹ）With the 4th filtrate（Ⅺ）, the 4th filtrate（Ⅺ）Middle addition 0.5-3.5mol/L sulfuric acid
The ammonium sulfate of magnesium, 0.5-5.3mol/L；Control magnesium phosphorus mol ratio 1.5-2.0:1, nitrogen phosphorus mol ratio 2-4:1,15-25min is stood,
It is filtrated to get the 5th filtrate（XIII）And ammoniomagnesium phosphate crystal, the 5th filtrate（XIII）Participate in pH regulation；
D, sorbing material attribute testing：By the second residue（Ⅴ）600-650 DEG C is carried out, 1-2h calcinings, using solid-to-liquid ratio 1：10
Adsorption bleaching, mixing speed 50-200r/min, 1-2h, pH=1- are carried out to the reactive gaudy red X 3B dye waste water that absorbance is 1
10；
E, product component is analyzed：XRD test analysis, ammonium magnesium phosphate crystal purity reach 97.0%, wherein 2% magnesium phosphate and hydrogen-oxygen
Change magnesium, 1% is the mixed phosphate of heavy metal, and ICP tests product heavy metal ion as shown by data：In product each heavy metal species from
Son reaches agricultural phosphate fertilizer standard, is used for agriculture slow-release phosphate fertilizer；
Described solid-to-liquid ratio is the ratio between solid masses and liquid volume, unit g/mL.
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