CN106882779A - A kind of method that phosphorus is reclaimed from city garbage burning flying ash - Google Patents
A kind of method that phosphorus is reclaimed from city garbage burning flying ash Download PDFInfo
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- CN106882779A CN106882779A CN201710178115.3A CN201710178115A CN106882779A CN 106882779 A CN106882779 A CN 106882779A CN 201710178115 A CN201710178115 A CN 201710178115A CN 106882779 A CN106882779 A CN 106882779A
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- flying dust
- incineration
- phosphorus
- reclaimed
- calcium chloride
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- 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
- C01B25/32—Phosphates of magnesium, calcium, strontium, or barium
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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Abstract
The invention discloses a kind of method that phosphorus compound is reclaimed from city garbage burning flying ash, its step：A. incineration of refuse flyash is fetched from municipal refuse incineration power factory, flying dust is modified with low-concentration hcl, remove part heavy metal, modified flying dust is filtered, take filter residue drying；B. leaching leaching is carried out to the filter residue dried in step a with hydrochloric acid, is obtained during P elements are discharged into supernatant in the form of the positive phosphorus acid ion；C. to the filtrate in step b, pH is adjusted with NaOH, is crystallized with calcium chloride, phosphate anion is precipitated in the form of calcium phosphate；D. precipitated product rinsing drying is obtained into solids of sedimentation, ultimate analysis determines that precipitated product is calcium phosphate.It is easy to implement the method, it is easy to operate, the phosphorus compound in incineration of refuse flyash can be reclaimed, set up the artificial phosphorus circulation canal of nature.For the recycling of incineration of refuse flyash provides a new way, be conducive to further studying the resource circulation utilization of incineration of refuse flyash.
Description
Technical field
The invention belongs to environmental technology field, it is more particularly to one kind and phosphorus compound is reclaimed from city garbage burning flying ash
Method, it be applied to city garbage burning flying ash recycling and chemical phosphorus recovery.
Background technology
Phosphorus is one of indispensable nutrient in vital movement, and it plays irreplaceable in the vital movement of cell
Effect.In biosphere, most phosphorus is one-way flow, does not have Efficient Cycle.Phosphate resource also thus turns into one
Kind unrenewable resource, standing crop is fewer and feweri, largely exploited in particular with industrial expansion phosphorus ore accelerate it is this
Loss.During environment (including rock, soil and water), biological and human circulation is participated in, it turns into again simultaneously causes phosphorus
A kind of important component of environmental pollution.With the yield of house refuse is increasing and to Disposal of Domestic requirement raising,
Burning method can turn into main flow processing mode in future, and this inevitably produces substantial amounts of incineration of refuse flyash.Waste incineration
Phosphorus in flying dust is (with P2O5Meter) content can reach 5%, be a kind of potential phosphor resource.Containing a large amount of in incineration of refuse flyash
Heavy metal, every country all regarded as danger wastes so that the treatment of incineration of refuse flyash is manipulated so for a disaster
Topic.Therefore therefrom reclaim phosphorus and set up artificial phosphorus circulation, one can be turned into rationally using the one of incineration of refuse flyash in future
Individual important directions.
In the last few years, as domestic and international researcher reclaims a series of researchs for carrying out to the phosphorus in waste water, currently used for
The technique that phosphorus is reclaimed from waste water mainly has the precipitation method, absorption method, bioanalysis etc..Contain substantial amounts of heavy metal among flying dust, make
The method for obtaining therefrom recovery phosphorus is relatively simple, and the precipitation method are optimal selections.The calcium phosphate of recovery can produce phosphorus as chemical fertilizer factory
The important phosphorus source of fertilizer.
The content of the invention
The present invention seeks to there are provided a kind of method that phosphorus compound is reclaimed from city garbage burning flying ash, raw material
It is easy to get, it is easy to implement the method, it is easy to operate, the phosphorus compound in incineration of refuse flyash can be reclaimed, set up the artificial phosphorus circulation of nature logical
Road.The recycling for being processed as incineration of refuse flyash provides a new way, is conducive to further studying waste incineration
The resource circulation utilization of flying dust.
In order to realize above-mentioned purpose, the present invention uses following technical measures：
A kind of method that phosphorus compound is reclaimed from city garbage burning flying ash, its step is：
A, flying dust pretreatment：Flying dust to obtaining is ground sieving (screen cloth of 180-210 mesh), obtains particle uniform
Flying dust, carry out that immersion is modified using hydrochloric acid, pH is 4.5-5.5, and solid-to-liquid ratio is 1:5, soak 10-14 hours, obtain a kind of
Flying dust A；
B, filtering：Pretreated flying dust A is filtered, filter residue is dried under the conditions of 118-122 DEG C, entered again
Row grinding sieving (screen cloth of 180-210 mesh), obtains evengranular modified flying dust B；
C, leaching：Taking a certain amount of (3-8g) flying dust B carries out leaching, adds the hydrochloric acid of 2mol/L, controls solid-to-liquid ratio 1:5, temperature
Degree control is in room temperature (20-25 DEG C, as follows), mixing speed 50-200r/min, mixing time 1.5-2.5h so that pre- place
Flying dust B after reason fully reacts with acid solution；
D, filtering：Abundant reacted solution is filtered using circulating water type vavuum pump, obtains supernatant C；
E, plus alkali regulation：Supernatant C is taken, pH is adjusted with NaOH, pH is 8.5-10.5, and Optimal pH is 9.5, at this
PH is strictly controlled in one step, recovery of pH during crystallization on product influences maximum；
F, plus crystallization of calcium chloride：After regulating pH, pH is 8.5-10.5, add calcium chloride crystallized, calcium chloride plus
It is that every 1 kilogram of flying dust B adds 85-95g calcium chloride to be crystallized to enter ratio, temperature control at 23-27 DEG C, optimal control temperature
It is 25 DEG C to spend, and mixing time is 13-17 minutes；
The treatment of G, crystallized product：Suction filtration is carried out to crystallization solution with circulating water type vavuum pump (SHZ-D (III)), is constantly added
Water is rinsed, and carries out suction filtration, and crystallized product is rinsed.Dried under the conditions of 103-107 DEG C, obtain pure solid and sink
Form sediment, using electron-microscope scanning and the fundamental property of X-ray diffraction analysis sediment, determine that product is calcium phosphate.
Described flying dust be collected in municipal refuse incineration power factory flue gas purification system obtained by fine particle, including with
The material produced during Chemical treatment flue gas, belongs to hazardous waste.
The present invention compared with prior art, has the advantages that following obvious protrusion：
(1) incineration of refuse flyash originally belongs to dangerous waste, deals with cumbersome, now use experimental technique recovery waste incineration
Phosphorus in flying dust, can mitigate harm of the incineration of refuse flyash to environment.
(2) treatment is modified to incineration of refuse flyash, the activity of flying dust can be changed, while part in flying dust can be removed
Soluble heavy metal.
(3) calcium phosphate is generated during being somebody's turn to do, ion solubility level constant is lower than cadmium phosphate, aluminum phosphate, the purity of crystallized product
It is high.
(4) calcium phosphate, as high-quality sustained release farmers' phosphate fertilizer, is good selection.
(5) present invention is applicable not only to the extraction recovery of sludge incineration ash, while being also applied for phosphorous mine tailing and part
The waste residue of phosphorus ore industry.
Brief description of the drawings
Fig. 1 is a kind of method block diagram that phosphorus compound is reclaimed from city garbage burning flying ash.
Wherein：1- flying dusts, 2- pretreatments, 3- filterings, 4- leachings, 5- filtering, 6- add alkali to adjust pH, 7- chlorination
Change calcium crystallization, the treatment of 8- crystallized products.
Specific embodiment
Embodiment 1：
The present invention is described in further detail below in conjunction with the accompanying drawings:
A kind of method that phosphorus compound is reclaimed from city garbage burning flying ash, its step is：
1. incineration of refuse flyash sampling：Flying dust used takes from Wuhan thing lake garbage incinerating power plant electrostatic precipitation during experiment
Device, sampling duration 10 hours, be ground for flying dust after terminating by sampling interval 1h/ times, single sampling amount 200g, sampling, mixes
Sieving (180 or 190 or 200 or 210 mesh), to ensure the uniformity of each element content in flying dust, obtains a kind of flying dust A；
2. pre-process：Ground incineration of refuse flyash A 200g are taken, adds the hydrochloric acid solution of 1000ml to be soaked, pH
Be 5, when the time be 2h, temperature keep room temperature, obtain evengranular modified flying dust B；
3. filter:After immersion terminates, suction filtration is carried out to soak with circulating water type vavuum pump, filter residue is under the conditions of 105 DEG C
Weight is dried to, filtrate is negligible with the phosphorus content that ammonium molybdate colorimetric method measures the inside, i.e., the phosphorus lost in preprocessing process
It is negligible.Detect phosphorus content in pretreated incineration of refuse flyash B is 34.68g/Kg.
4. leaching：Take the flying dust B 5g after pretreatment drying, solid-to-liquid ratio 1:5, concentration of hydrochloric acid 2mol/L, rotating speed 100rpm,
20 DEG C of normal temperature process 2h.
5. filter：The leaching liquor of filtration step 4 obtains filtrate, and measuring the phosphorus content in filtrate with ammonium molybdate colorimetric method is
The dissolution rate of 0.15g, i.e. phosphorus is 86.5%.
6. alkali regulation is added：Take the filtrate of step 5, use sodium hydrate regulator solution pH, pH be 8.5 or 9 or 9.5 or 10 or
Between 10.5, the Optimal pH obtained by experiment is 9.5, pH is strictly controlled in this step, recovery of pH during crystallization to product
Influence is maximum.
7. crystallization of calcium chloride is added：After regulating pH, pH is 8.5 or 9 or 9.5 or 10 or 10.5, adds calcium chloride to be tied
Crystalline substance, the optimum condition obtained by experiment is：The dosage of calcium chloride is 80g/Kg, and at 20 DEG C, the stirring reaction time is temperature control
15min, mixing speed be 100rpm under conditions of carry out crystallization of calcium chloride.
8. the treatment of crystallized product：Suction filtration is carried out to crystallization solution with circulating water type vavuum pump, constantly add water flushing, goes forward side by side
Row suction filtration, rinses to crystallized product.Dried under the conditions of 105 DEG C, obtain pure solids of sedimentation, using electron-microscope scanning and
The fundamental property of X-ray diffraction analysis sediment, determines that product is calcium phosphate.
Result shows：In Leaching Experiments, flying dust quality is 1 with hydrochloric acid volume:5, concentration of hydrochloric acid is 2mol/L, and rotating speed is
100rpm, the dissolution of phosphorus is optimal during 20 DEG C of normal temperature treatment 2h, has reached 86.5%；In crystallization experiment, NaOH is used
Regulation pH value of solution is 9.5, and the dosage of calcium chloride is 80g/Kg, temperature control at 20 DEG C, when mixing time is 15min, phosphoric acid
The percent crystallization in massecuite highest of radical ion, has substantially achieved 98%.0.77g calcium phosphate crystal products are obtained after drying, ammonium molybdate ratio is used
Color method measures the substantially all crystalline deposit of phosphorus in filtrate；ICP tests product heavy metal ion as shown by data, various in product
Heavy metal ion can reach agricultural phosphate fertilizer standard.XRD test analysis, the purity of calcium phosphate can reach 97%, can be as
Agriculture slow-release phosphate fertilizer is used.This example has reclaimed in incineration of refuse flyash 86.5% P, and the incineration of refuse flyash of 1 ton for the treatment of can
Obtain the calcium phosphate crystal product of 154Kg.
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 for wherein illustrating 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 done by scope of the invention and modification all should scope of patent protection of the invention it
Row.
Claims (1)
1. a kind of method that phosphorus compound is reclaimed from city garbage burning flying ash, its step is：
A, flying dust pretreatment：Flying dust to obtaining is ground sieving, obtains evengranular flying dust, is soaked using hydrochloric acid
Modified, pH is 4.5-5.5, and solid-to-liquid ratio is 1:5, soak 10-14 hours, obtain a kind of flying dust A；
B, filtering：Pretreated flying dust A is filtered, filter residue is dried under the conditions of 118-122 DEG C, ground again
Honed sieve, obtains evengranular modified flying dust B；
C, leaching：Taking flying dust B carries out leaching, adds the hydrochloric acid of 2mol/L, controls solid-to-liquid ratio 1:5, temperature control is in room temperature, stirring
Speed 50-200r/min, mixing time 1.5-2.5h so that pretreated flying dust B fully reacts with acid solution；
D, filtering：Reacted solution is filtered using circulating water type vavuum pump, obtains supernatant C；
E, plus alkali regulation：Supernatant C is taken, pH is adjusted with NaOH, pH is 8.5-10.5；
F, plus crystallization of calcium chloride：After regulation pH, pH is 8.5-10.5, adds calcium chloride to be crystallized, the additional proportion of calcium chloride
It is that every 1 kilogram pretreated flying dust B adds 85-95g calcium chloride to be crystallized, temperature control is in 23-27 DEG C, mixing time
It is 13-17 minutes；
The treatment of G, crystallized product：Suction filtration is carried out to crystallization solution with circulating water type vavuum pump, constantly add water flushing, and is taken out
Filter, rinses to crystallized product, is dried under the conditions of 103-107 DEG C, pure solids of sedimentation is obtained, using electron-microscope scanning
With X-ray diffraction analysis sediment, determine that product is calcium phosphate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201710178115.3A CN106882779B (en) | 2017-03-23 | 2017-03-23 | A method of recycling phosphorus from city garbage burning flying ash |
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| CN201710178115.3A CN106882779B (en) | 2017-03-23 | 2017-03-23 | A method of recycling phosphorus from city garbage burning flying ash |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111440011A (en) * | 2020-03-13 | 2020-07-24 | 中国科学院武汉岩土力学研究所 | Method for preparing phosphate fertilizer from municipal sludge |
| CN111548197A (en) * | 2020-05-20 | 2020-08-18 | 四川大学 | Method for recovering calcium phosphate fertilizer from sludge incineration bottom ash |
| WO2022022090A1 (en) * | 2020-07-29 | 2022-02-03 | 同济大学 | Method for recovering vivianite from sludge incineration ash |
| CN114436232A (en) * | 2022-02-14 | 2022-05-06 | 安徽理工大学 | Method for preparing hydroxyapatite by using waste incineration ash |
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| CN1947872A (en) * | 2006-11-09 | 2007-04-18 | 上海大学 | Water washing pretreatment method for making fly-ash from incineration harmless |
| CN100506405C (en) * | 2006-02-17 | 2009-07-01 | 清华大学 | Chemical process of stabilizing fly ash from incinerating city garbage |
| CN105110506A (en) * | 2015-08-28 | 2015-12-02 | 浙江省环境保护科学设计研究院 | Acid mine drainage/refuse incineration fly ash coupled stabilization treatment method |
| CN106430136A (en) * | 2016-09-08 | 2017-02-22 | 张国闽 | Method for recovering phosphorus and removing heavy metals from sludge separate incineration ash residues |
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Patent Citations (4)
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| CN100506405C (en) * | 2006-02-17 | 2009-07-01 | 清华大学 | Chemical process of stabilizing fly ash from incinerating city garbage |
| CN1947872A (en) * | 2006-11-09 | 2007-04-18 | 上海大学 | Water washing pretreatment method for making fly-ash from incineration harmless |
| CN105110506A (en) * | 2015-08-28 | 2015-12-02 | 浙江省环境保护科学设计研究院 | Acid mine drainage/refuse incineration fly ash coupled stabilization treatment method |
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| 薛勇刚等: "磷回收技术及其在污泥资源化领域的研究进展", 《环境科学与技术》 * |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111440011A (en) * | 2020-03-13 | 2020-07-24 | 中国科学院武汉岩土力学研究所 | Method for preparing phosphate fertilizer from municipal sludge |
| CN111548197A (en) * | 2020-05-20 | 2020-08-18 | 四川大学 | Method for recovering calcium phosphate fertilizer from sludge incineration bottom ash |
| WO2022022090A1 (en) * | 2020-07-29 | 2022-02-03 | 同济大学 | Method for recovering vivianite from sludge incineration ash |
| CN114436232A (en) * | 2022-02-14 | 2022-05-06 | 安徽理工大学 | Method for preparing hydroxyapatite by using waste incineration ash |
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| CN106882779B (en) | 2018-12-25 |
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