CN108910849A - A method of circulation extracts phosphorus from sludge ash - Google Patents
A method of circulation extracts phosphorus from sludge ash Download PDFInfo
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- CN108910849A CN108910849A CN201810811884.7A CN201810811884A CN108910849A CN 108910849 A CN108910849 A CN 108910849A CN 201810811884 A CN201810811884 A CN 201810811884A CN 108910849 A CN108910849 A CN 108910849A
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- phosphorus
- sludge ash
- sludge
- ash
- sulfuric acid
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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
- C01B25/18—Phosphoric acid
- C01B25/22—Preparation by reacting phosphate-containing material with an acid, e.g. wet process
- C01B25/222—Preparation by reacting phosphate-containing material with an acid, e.g. wet process with sulfuric acid, a mixture of acids mainly consisting of sulfuric acid or a mixture of compounds forming it in situ, e.g. a mixture of sulfur dioxide, water and oxygen
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Abstract
The invention discloses a kind of to recycle the method for extracting phosphorus from sludge ash, and this method is first once extracted with sulfuric acid solution using sludge incineration ash as raw material, then by extracting solution and concentrated sulfuric acid solution according to 28.8:1.2~28.4:1.6 volume ratio is hybridly prepared into new extractant, extracts to remaining sludge ash；As needed, sludge ash can be divided into more parts, repeatedly extracted, extractant used when primary extraction is mixed by the extracting solution after the completion of preceding primary extraction with concentrated sulfuric acid solution afterwards.It is used in the present invention using extracting solution as extractant, the discharge of waste liquid can be greatly decreased, and after circulation is extracted, the recovery rate of phosphorus can be more than 96% in sludge ash, the concentration of phosphorus is more than 21~23g/L in final extracting solution, can effectively solve in the prior art the technical issues of phosphorus recovery rate is low, reagent consumption amount is big and generates a large amount of waste liquids.
Description
Technical field
The invention belongs to sewage treatment plant's technical field of resource recovery, and in particular to one kind circulation from sludge ash extracts phosphorus
Method.
Background technique
Phosphorus is one of the essential elements that all life entities are depended on for existence, is played in terms of eucaryotic cell structure and cell function important
Effect.With the development of industrial or agricultural, the mankind increasingly increase the demand of rock phosphate in powder, and phosphorus is a kind of unidirectional in biosphere
The element of flowing, the contradiction being further exacerbated by between demand and supply.
The excess sludge recycling phosphorus that municipal sewage treatment process generates has very big potentiality.Excess sludge obtains after burning
The sludge ash for being 5%~10% to phosphorus content, it is suitable with the average content of phosphorus in Chinese phosphorus ore, have and proposes phosphorus value.
At this stage using the mode that phosphorus in more sludge ash extracts be using sulfuric acid or nitric acid high liquid-solid ratio (>15mL/
G) phosphorus in sludge ash is extracted under, still, not only the recovery rate of phosphorus is low in this way, but also can generate a large amount of
Waste liquid is unfavorable for the protection of environment.
Summary of the invention
For the above-mentioned prior art, the present invention provides a kind of method that circulation extracts phosphorus from sludge ash, is mentioned with solving phosphorus
Take the technical issues of rate is low, reagent consumption amount is big and generates a large amount of waste liquids.
In order to achieve the above object, the technical scheme adopted by the invention is that：One kind is provided and recycles extraction from sludge ash
The method of phosphorus, includes the following steps：
(1) sludge incineration ash is taken, is sieved with 100 mesh sieve after ball milling；
(2) sulfuric acid solution that mass fraction is 7%~13% is heated to 25~45 DEG C, then with sludge ash by 2~
The liquid-solid ratio of 5mL/g mixes, and obtains slurry；
(3) slurry is placed in stirring instrument, is stirred to react 30min under the conditions of 25~45 DEG C, >=150rmp, be then added
Deionized water terminates reaction, then filters to the slurry after reaction, and filtered sludge ash filter cake wash with distilled water, cleans
Liquid merges to obtain extracting solution with filtrate；
(4) sulfuric acid solution that extracting solution and mass fraction are 98% is pressed 28.8:1.2~28.4:1.6 volume ratio is mixed
It closes, obtains extractant, with the sulfuric acid solution in extractant step of replacing (2), the side in step (2)~(3) is pressed to excess sludge ash
Method extracts；
(5) step (4) n times are repeated, complete to extract；N-th is extracted the extracting solution after extractant used is extracted by N-1 times and is pressed
Method in step (4) is formulated.
Based on the above technical solution, the present invention can also be improved as follows.
Further, sludge incineration ash is derived from urban domestic sewage sludge incineration plant.
Further, the mass fraction of sulfuric acid solution used is 10% in step (2).
Further, the liquid-solid ratio of sulfuric acid solution and sludge ash is 3mL/g in step (2).
Further, it is 25 DEG C that temperature is stirred to react in step (3), stirring rate 150rmp.
Further, 8≤N≤12 in step (5).
The beneficial effects of the invention are as follows：
1. the phosphorus of extracting method of the invention using the sludge incineration ash of city domestic sewage treatment plant as raw material, in the raw material
Content is suitable with common rock phosphate in powder, and the exploitation of rock phosphate in powder can be not only reduced using it as raw material, avoids large-scale ecology broken
It is bad, and do not have to carry out complicated pre-treatment, extracting difficulty reduces, while realizing the recycling of sludge ash, avoids at sludge ash
Set improper pollute the environment.
2. the present invention repeatedly extracts the phosphorus in sludge ash using circulating extraction method, occur in the extraction process of phosphorus
Following reaction：
Ca19Fe2(PO4)14+19SO4 2-+42H++xH2O→19CaSO4·xH2O↓+14H3PO4+2Fe2+
By reaction equation it is found that first sulfuric acid is used to extract as extractant, precipitating not soluble in water can be generated, promotes reaction
It moves right, the amount of precipitation of phosphorus increases, and the recovery rate of phosphorus increases in sludge ash.When carrying out second extraction, extractant is by extracting solution
It is formed with sulfuric acid solution mixed preparing, phosphorus is present in extracting solution in the form of phosphoric acid, can reduce the pH value of extractant, metal phosphorus
Hydrochlorate is easier to dissolve at the low ph, promotes the precipitation of phosphorus, the recovery rate of phosphorus further increases；And extracting solution conduct
Extractant uses, and the dosage of extractant can be greatly reduced, avoid generating excessive waste liquid.
3. the present invention is during the extraction process, the liquid-solid ratio of extractant and sludge ash is controlled within the scope of 2~5mL/g, and liquid is solid
Relatively low, extractant can be sufficiently with sludge ash haptoreaction, and conducive to the precipitation of phosphorus, recovery rate increases.
Specific embodiment
The present invention proposes a kind of new phosphorus extracting method, this method includes following step on the basis of existing acid extracts phosphorus
Suddenly：
(1) sludge incineration ash is taken, is put into ball mill and carries out ball milling, 100 meshes of the powder after ball milling are sieved；Consider
Sludge phosphorus content with higher after being burned to city domestic sewage treatment plant, while raw material is easy to get, the sludge in the present invention
Burning ash is preferentially obtained from city domestic sewage treatment plant.
(2) it is spare to prepare the sulfuric acid solution that mass fraction is 7%~13%.It is by heating equipment that prepared sulfuric acid is molten
Liquid is heated to 25~45 DEG C, and then the sulfuric acid after heating is quickly poured into the container equipped with sludge ash, the sulfuric acid solution poured into
Solid-liquid ratio with sludge ash in container is 2~5mL/g, and starts stirring instrument and be stirred, and controls stirring rate >=150rmp,
Following reaction occurs in whipping process, in conical flask：
Ca19Fe2(PO4)14+19SO4 2-+42H++xH2O→19CaSO4·xH2O↓+14H3PO4+2Fe2+
After being stirred to react 30min, stirring instrument is closed, pours into a certain amount of deionized water dilution cooling into container immediately
Make reaction terminating, then carries out vacuum filtration separated sludge mortar；Filter the sludge ash filter cake distilled water that is retained down into
Row cleaning, obtains extracting solution after cleaning solution is merged with filtrate；Sludge ash filter cake after cleaning is dried with drying unit.
(3) sulfuric acid solution that extracting solution and mass fraction are 98% is pressed 28.8:1.2~28.4:1.6 volume ratio is mixed
It closes, preparation obtains extractant, with the sulfuric acid solution in extractant step of replacing (2), presses in step (2) to remaining sludge ash
Method extracts again；
(4) step (3) n times are repeated, complete to extract；N-th is extracted the extracting solution after extractant used is extracted by N-1 times and is pressed
Method in step (2) is formulated.
Specific embodiments of the present invention will be described in detail combined with specific embodiments below.
Embodiment one
A method of circulation extracts phosphorus from sludge ash, includes the following steps：
(1) sludge incineration ash in city domestic sewage treatment plant is taken, is sieved with 100 mesh sieve after ball milling；
(2) sulfuric acid solution that mass fraction is 10% is heated to 25 DEG C, it is then mixed by the liquid-solid ratio of 3mL/g with sludge ash
It closes, obtains slurry；
(3) slurry is placed in stirring container, is stirred to react 30min under the conditions of 25 DEG C, 150rmp, then be added go from
Sub- water terminates reaction, then filters to the slurry after reaction, filtered sludge ash filter cake wash with distilled water, cleaning solution with
Filtrate merges to obtain extracting solution；
(4) sulfuric acid solution that extracting solution and mass fraction are 98% is pressed 28.8:1.2 volume ratio mixing, prepares and extracts
Agent is mentioned excess sludge ash by the method in step (2)~(3) with the sulfuric acid solution in extractant step of replacing (2)
It takes；
(5) it repeats step (4) 8 times, completes to extract；Wherein, n-th extracts mentioning after extractant used is extracted by N-1 times
Liquid is taken to be formulated by the method in step (4), extracting solution and quality after being extracted such as the 8th extraction extractant used by 7 times
The sulfuric acid solution that score is 98% presses 28.8:1.2 volume ratio mixes.
Embodiment two
A method of circulation extracts phosphorus from sludge ash, includes the following steps：
(1) sludge incineration ash in city domestic sewage treatment plant is taken, is sieved with 100 mesh sieve after ball milling；
(2) sulfuric acid solution that mass fraction is 7% is heated to 45 DEG C, it is then mixed by the liquid-solid ratio of 4mL/g with sludge ash
It closes, obtains slurry；
(3) slurry is placed in stirring container, is stirred to react 30min under the conditions of 45 DEG C, 200rmp, then be added go from
Sub- water terminates reaction, then filters to the slurry after reaction, filtered sludge ash filter cake wash with distilled water, cleaning solution with
Filtrate merges to obtain extracting solution；
(4) sulfuric acid solution that extracting solution and mass fraction are 98% is pressed 28.4:1.2 volume ratio mixing, prepares and extracts
Agent is mentioned excess sludge ash by the method in step (2)~(3) with the sulfuric acid solution in extractant step of replacing (2)
It takes；
(5) it repeats step (4) 9 times, completes to extract；Wherein, n-th extracts mentioning after extractant used is extracted by N-1 times
Liquid is taken to be formulated by the method in step (4), extracting solution and quality after being extracted such as the 9th extraction extractant used by 8 times
The sulfuric acid solution that score is 98% presses 28.4:1.2 volume ratio mixes.
Embodiment three
A method of circulation extracts phosphorus from sludge ash, includes the following steps：
(1) sludge incineration ash in city domestic sewage treatment plant is taken, is sieved with 100 mesh sieve after ball milling；
(2) sulfuric acid solution that mass fraction is 13% is heated to 30 DEG C, it is then mixed by the liquid-solid ratio of 5mL/g with sludge ash
It closes, obtains slurry；
(3) slurry is placed in stirring container, is stirred to react 30min under the conditions of 30 DEG C, 300rmp, then be added go from
Sub- water terminates reaction, then filters to the slurry after reaction, filtered sludge ash filter cake wash with distilled water, cleaning solution with
Filtrate merges to obtain extracting solution；
(4) sulfuric acid solution that extracting solution and mass fraction are 13% is pressed 28.4:1.6 volume ratio mixing, prepares and extracts
Agent is mentioned excess sludge ash by the method in step (2)~(3) with the sulfuric acid solution in extractant step of replacing (2)
It takes；
(5) it repeats step (4) 10 times, completes to extract；Wherein, n-th extracts mentioning after extractant used is extracted by N-1 times
Liquid is taken to be formulated by the method in step (4), extracting solution and quality after being extracted such as the 10th extraction extractant used by 9 times
The sulfuric acid solution that score is 98% presses 28.4:1.6 volume ratio mixes.
Example IV
A method of circulation extracts phosphorus from sludge ash, includes the following steps：
(1) sludge incineration ash in city domestic sewage treatment plant is taken, is sieved with 100 mesh sieve after ball milling；
(2) sulfuric acid solution that mass fraction is 7% is heated to 30 DEG C, it is then mixed by the liquid-solid ratio of 3mL/g with sludge ash
It closes, obtains slurry；
(3) slurry is placed in stirring container, is stirred to react 30min under the conditions of 30 DEG C, 350rmp, then be added go from
Sub- water terminates reaction, then filters to the slurry after reaction, filtered sludge ash filter cake wash with distilled water, cleaning solution with
Filtrate merges to obtain extracting solution；
(4) sulfuric acid solution that extracting solution and mass fraction are 7% is pressed 28.8:1.6 volume ratio mixing, prepares and extracts
Agent is mentioned excess sludge ash by the method in step (2)~(3) with the sulfuric acid solution in extractant step of replacing (2)
It takes；
(5) it repeats step (4) 12 times, completes to extract；Wherein, n-th extracts mentioning after extractant used is extracted by N-1 times
Liquid is taken to be formulated by the method in step (4), extracting solution and matter after being extracted such as the 12nd extraction extractant used by 11 times
It measures the sulfuric acid solution that score is 98% and presses 28.8:1.6 volume ratio mixes.
Using the method in the present invention, the recovery rate of phosphorus is up to 96% or more, and the concentration of phosphorus is more than 21 in final extracting solution
~23g/L can substantially extract the phosphorus in sludge ash, compared with the existing technology in extracting method, not only reduce waste liquid
Discharge amount, can also reduce the yield of rock phosphate in powder, be a kind of environment amenable extracting mode.
Although be described in detail to a specific embodiment of the invention in conjunction with the embodiments, should not be construed as to this
The restriction of the protection scope of patent.In range described by claims, those skilled in the art are without creative work
The various modifications and deformation that can make still belong to the protection scope of this patent.
Claims (6)
1. a kind of method that circulation extracts phosphorus from sludge ash, which is characterized in that include the following steps：
(1) sludge incineration ash is taken, is sieved with 100 mesh sieve after ball milling；
(2) sulfuric acid solution that mass fraction is 7%~13% is heated to 25~45 DEG C, then with sludge ash by 2~5mL/g's
Liquid-solid ratio mixing, obtains slurry；
(3) by slurry be placed in stirring instrument in, be stirred to react 30min under the conditions of 25~45 DEG C, >=150rmp, then be added go from
Sub- water terminates reaction, then filters to the slurry after reaction, filtered sludge ash filter cake wash with distilled water, cleaning solution with
Filtrate merges to obtain extracting solution；
(4) sulfuric acid solution that extracting solution and mass fraction are 98% is pressed 28.8:1.2~28.4:1.6 volume ratio mixing, obtains
Extractant is carried out excess sludge ash by the method in step (2)~(3) with the sulfuric acid solution in extractant step of replacing (2)
It extracts；
(5) step (4) n times are repeated, complete to extract；N-th extracts the extracting solution after extractant used is extracted by N-1 times and presses step
(4) method in is formulated.
2. the method according to claim 1 that circulation extracts phosphorus from sludge ash, it is characterised in that：The sludge incineration ash
It is derived from urban domestic sewage sludge incineration plant.
3. the method according to claim 1 that circulation extracts phosphorus from sludge ash, it is characterised in that：It is used in step (2)
The mass fraction of sulfuric acid solution is 10%.
4. the method according to claim 1 that circulation extracts phosphorus from sludge ash, it is characterised in that：Sulfuric acid in step (2)
The liquid-solid ratio of solution and sludge ash is 3mL/g.
5. the method according to claim 1 that circulation extracts phosphorus from sludge ash, it is characterised in that：Stirring in step (3)
Reaction temperature is 25 DEG C, stirring rate 150rmp.
6. the method according to claim 1 that circulation extracts phosphorus from sludge ash, it is characterised in that：8≤N in step (5)
≤12。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201810811884.7A CN108910849B (en) | 2018-07-23 | 2018-07-23 | Method for circularly extracting phosphorus from sludge ash |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810811884.7A CN108910849B (en) | 2018-07-23 | 2018-07-23 | Method for circularly extracting phosphorus from sludge ash |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111548197A (en) * | 2020-05-20 | 2020-08-18 | 四川大学 | Method for recovering calcium phosphate fertilizer from sludge incineration bottom ash |
| CN111646674A (en) * | 2020-04-30 | 2020-09-11 | 中国环境科学研究院 | Method for releasing and recovering phosphorus in sludge |
| EP3770113A1 (en) * | 2019-07-25 | 2021-01-27 | Técnicas Reunidas, S.A. | Process for preparing technical grade phosphoric acid from sewage sludge ash |
| WO2022022090A1 (en) * | 2020-07-29 | 2022-02-03 | 同济大学 | Method for recovering vivianite from sludge incineration ash |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP3770113A1 (en) * | 2019-07-25 | 2021-01-27 | Técnicas Reunidas, S.A. | Process for preparing technical grade phosphoric acid from sewage sludge ash |
| EP4206125A1 (en) * | 2019-07-25 | 2023-07-05 | Técnicas Reunidas, S.A. | Process for preparing technical grade phosphoric acid from sewage sludge ash |
| CN111646674A (en) * | 2020-04-30 | 2020-09-11 | 中国环境科学研究院 | Method for releasing and recovering phosphorus in 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 |
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