CN111646674A - Method for releasing and recovering phosphorus in sludge - Google Patents
Method for releasing and recovering phosphorus in sludge Download PDFInfo
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- CN111646674A CN111646674A CN202010363061.XA CN202010363061A CN111646674A CN 111646674 A CN111646674 A CN 111646674A CN 202010363061 A CN202010363061 A CN 202010363061A CN 111646674 A CN111646674 A CN 111646674A
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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
- C02F11/12—Treatment of sludge; Devices therefor by de-watering, drying or thickening
- C02F11/15—Treatment of sludge; Devices therefor by de-watering, drying or thickening by treatment with electric, magnetic or electromagnetic fields; by treatment with ultrasonic waves
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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
- C01B25/01—Treating phosphate ores or other raw phosphate materials to obtain phosphorus or phosphorus compounds
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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
- C02F11/12—Treatment of sludge; Devices therefor by de-watering, drying or thickening
- C02F11/14—Treatment of sludge; Devices therefor by de-watering, drying or thickening with addition of chemical agents
- C02F11/143—Treatment of sludge; Devices therefor by de-watering, drying or thickening with addition of chemical agents using inorganic substances
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F23—COMBUSTION APPARATUS; COMBUSTION PROCESSES
- F23G—CREMATION FURNACES; CONSUMING WASTE PRODUCTS BY COMBUSTION
- F23G5/00—Incineration of waste; Incinerator constructions; Details, accessories or control therefor
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F23—COMBUSTION APPARATUS; COMBUSTION PROCESSES
- F23G—CREMATION FURNACES; CONSUMING WASTE PRODUCTS BY COMBUSTION
- F23G5/00—Incineration of waste; Incinerator constructions; Details, accessories or control therefor
- F23G5/02—Incineration of waste; Incinerator constructions; Details, accessories or control therefor with pretreatment
- F23G5/04—Incineration of waste; Incinerator constructions; Details, accessories or control therefor with pretreatment drying
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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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- Treatment Of Sludge (AREA)
Abstract
The invention discloses a method for releasing and recovering phosphorus in sludge, which mainly comprises the following steps: adding a flocculating agent into the sludge, stirring, performing ultrasonic pretreatment, and finally performing mechanical dehydration; drying the dewatered sludge, grinding the dewatered sludge by a grinder to prepare dry sludge for later use; incinerating the prepared dry sludge to obtain sludge incineration ash, putting the incineration ash into a container, adding an extracting agent, and performing centrifugal treatment under a certain liquid-solid ratio condition to obtain sludge supernatant rich in a large amount of phosphorus; adding the obtained supernatant rich in a large amount of phosphorus into a reactor for fine purification treatment; taking refined and pure treatmentThe supernatant is used as stock solution and put in a container, after the pH is adjusted, MgCl is added2·6H2And O to obtain the phosphorization precipitate, and the method improves the recovery and utilization rate of phosphorus in the sludge from the source and is suitable for wide popularization.
Description
Technical Field
The invention relates to the technical field of sludge recycling, in particular to a method for releasing and recycling phosphorus in sludge.
Background
Phosphorus is an important non-metallic mineral resource which is difficult to regenerate, and is one of the most important elements for life activities. At present, the reserves of 27 hundred million standard phosphate ores in China are only enough to maintain the reuse of China for about 70 years, and the reserves also contain over 90 percent of non-phosphorus-rich ores. If the method is only calculated by the phosphorus reserves of rich phosphate rocks, the method can only be used for 10 to 15 years in China.
After the sludge is incinerated at high temperature, about 170 million of incineration ash is generated in the world every year, and after the phosphorus-rich sludge is dehydrated and incinerated, the phosphorus content in the incineration ash can reach 8% -10%, and the incineration ash can replace natural phosphate ore. However, most of the generated incineration ash is buried, the part capable of being recycled is used as raw materials for sintering bricks, producing clay substitutes and cement, and the like, wherein valuable phosphate is not reasonably utilized, and the phosphorus recovered from the sludge incineration ash can be used as a source for producing fertilizers and other phosphate products, so that the problem of shortage of phosphorus resources at present can be relieved.
The key point of recovering phosphorus from sludge incineration ash is to leach the phosphorus from the sludge incineration ash, the incineration ash is generally treated by a wet chemical method, common leaching agents comprise inorganic acid, alkali, organic acid, chelating agent and the like, the wet chemical method has a relatively simple leaching process and less loss, and the leaching efficiency of the phosphorus depends on the type, concentration, liquid-solid ratio, sludge incineration temperature and the like of the leaching agent. The inorganic acid can leach 84.3-100.0% of phosphorus, so that the method is widely applied.
Disclosure of Invention
In order to solve the technical problems, the invention provides a method for releasing and recovering phosphorus in sludge.
The technical points of the invention are as follows:
a method for releasing and recovering phosphorus in sludge mainly comprises the following steps:
s1, selecting a part of sludge of a sludge treatment plant, adding a flocculating agent into the selected sludge, stirring the sludge added with the flocculating agent to accelerate the flocculation speed, setting the stirring speed to be 200r/min, stirring for 10-25min, performing ultrasonic pretreatment on the stirred sludge, mechanically dehydrating the sludge after ultrasonic treatment to remove interstitial water and capillary water in the sludge, and breaking cell walls of biological cells in the sludge after ultrasonic pretreatment of the sludge, so that the improvement of the biodegradability of the sludge is beneficial to subsequent dehydration;
s2, drying the dewatered sludge after mechanical dewatering at 105 ℃ for 12h, removing the adsorbed water and the water inside the sludge, grinding the sludge into powder of 100 meshes by a grinder to prepare dry sludge for later use, wherein the dry sludge is convenient for subsequent incineration, and when the dry sludge is ground into powder and then incinerated, organic phosphorus in the sludge can be completely decomposed, and the total phosphorus almost consists of inorganic phosphorus and is easier to be leached by acid;
s3, placing the prepared dry sludge in a crucible, placing the crucible in a muffle furnace, setting the temperature to 600--1The lixiviant reacts for 2 hours at normal temperature under the condition of 15-150mL/g liquid-solid ratio, and then is subjected to centrifugal treatment to obtain sludge supernatant rich in a large amount of phosphorus, the large amount of phosphorus is released into the supernatant, the subsequent recovery of the phosphorus in the supernatant is convenient, the cost is saved for the conventional method for directly recovering the phosphorus in sewage, and the recovery rate of the phosphorus recovered in the supernatant is better;
s4, adding the obtained sludge supernatant rich in a large amount of phosphorus into a reactor for fine purification treatment, setting pulse voltage of 20Kv and pulse frequency of 200-300Hz, placing the upper electrode plate and the lower electrode plate in the supernatant, setting the distance between the upper electrode plate and the lower electrode plate to be 8mm, wherein the supernatant after pulse treatment is more fine and pure, and the phosphorus content in the supernatant is higher;
s5, taking the supernatant after S4 fine purification as stock solution, putting the stock solution into a container, adjusting the pH value of the stock solution to 8-11, adding MgCl with the ratio of n (Mg) to n (P) of 0.8-22·6H2O, at 200r/min-1Reacting for 24 hours under stirring, and then reacting at 4000 r.min-1Centrifuging for 10min, and removing supernatant to obtain the final product.
Furthermore, in the step S3, the residue left after centrifugation is continuously washed for multiple times by secondary deionized water, and then returned to the crucible, and then dried, burned and centrifuged, so that the resource waste is reduced.
Furthermore, when the residual residue after centrifugation in S3 is subjected to secondary incineration, the temperature is raised to 1200 ℃, after the residual residue is cooled, an extracting agent is added, the mixture reacts for 0.5 to 1 hour at normal temperature and then is subjected to centrifugal treatment to obtain a supernatant, and phosphide crystals can also be obtained from the supernatant after secondary separation.
Further, the leaching agent in S3 is selected from H2SO4HCL and HNO3One of them.
Furthermore, when the supernatant is removed in S5, the supernatant is discharged in a mode of upper water outlet, and the water outlet is sealed by a 0.45um filter membrane, so that the loss of phosphide precipitate is prevented, and the phosphide precipitate is separated more quickly.
Further, in S1, the ultrasonic frequency is set to be 20-100Hz, the ultrasonic treatment time is set to be 10min, and low-frequency sound waves can improve the biodegradability of the sludge and ensure that beneficial components in the sludge are not damaged.
Compared with the prior art, the invention has the beneficial effects that:
first, the invention selects H2SO4HCL and HNO3The phosphorus in the incineration ash is leached, the phosphorus leaching rate is improved to the maximum extent by controlling the incineration temperature of the sludge, the concentration of the leaching agent and the liquid-solid ratio, the release rate of the phosphorus reaches over 80 percent under specific reaction conditions, and a foundation is laid for the maximum recovery of the phosphorus.
Secondly, the sludge is subjected to ultrasonic pretreatment, the dehydration performance and the biodegradability of the sludge are improved, the sludge is dried and incinerated, and most of phosphorus in the sludge is converted into inorganic phosphorus after high-temperature incineration, so that the inorganic phosphorus is more easily leached by acid. When the temperature is 900 ℃, the TP release rate of the sludge incineration ash is also the highest and reaches 85.28%, and the content of phosphate radicals in the supernatant is more than 80%, so that the recovery of phosphorus is easy.
Thirdly, in the prior art, most of the generated incineration ash is buried, so that huge resource waste is generated, and the utilization value of the sludge ash cannot be exerted.
Detailed Description
The first embodiment is as follows:
a method for releasing and recovering phosphorus in sludge mainly comprises the following steps:
s1, selecting a part of sludge of a sludge treatment plant, adding a polysilicate ferric flocculant into the selected sludge according to a feeding ratio of 3kg/t, stirring the sludge added with the flocculant to accelerate the flocculation speed, setting the stirring speed to be 200r/min and the stirring time to be 10min, performing ultrasonic pretreatment on the stirred sludge, setting the ultrasonic frequency to be 100Hz and the ultrasonic treatment time to be 10min, and mechanically dehydrating the sludge after the ultrasonic pretreatment to remove interstitial water and capillary water in the sludge and enable the water content in the sludge to be 65%;
s2, drying the dewatered sludge subjected to mechanical dewatering for 12 hours at 105 ℃, removing adsorbed water and water inside the sludge, and grinding the sludge into powder of 100 meshes by a grinder to prepare dry sludge for later use;
s3, placing the prepared dry sludge into a crucible, placing the crucible into a muffle furnace, setting the temperature to 600 ℃ for incineration for 2 hours to obtain sludge incineration ash, cooling the incineration ash to room temperature, placing the sludge incineration ash into a container, and adding 0.2 mol.L-1H of (A) to (B)2SO4Lixiviant at 60mL g-1Reacting at normal temperature for 2h under the condition of liquid-solid ratio, centrifuging to obtain sludge supernatant rich in a large amount of phosphorus, continuously washing residues left after centrifuging for multiple times by using secondary deionized water, returning the residues to a crucible, drying, incinerating and centrifuging the residues, raising the temperature to 1200 ℃ when carrying out secondary incineration on the residues left after centrifuging in S3, cooling the residues, and adding 0.1 mol.L-1H2SO4Lixiviant, reacting at normal temperature for 0.5 hr, centrifuging to obtain supernatant, mixing with the supernatant,PO pairs in supernatant by this example4 3-P concentration was tested and the data were: 32.02mg g-1;
S4, adding the obtained sludge supernatant rich in a large amount of phosphorus into a reactor for fine purification: setting pulse voltage of 20Kv and pulse frequency of 200Hz, placing the upper electrode plate and the lower electrode plate in the supernatant, and setting the distance between the upper electrode plate and the lower electrode plate to be 8 mm;
s5, taking the supernatant after S4 fine purification treatment as stock solution, putting the stock solution into a container, adjusting the pH value of the stock solution to 8.5, adding MgCl with the ratio of n (Mg) to n (P) being 1.22·6H2O, at 200r/min-1Reacting for 24 hours under stirring, and then reacting at 4000 r.min-1Centrifuging for 10min, sealing the water outlet by adopting a 0.45um filter membrane, discharging supernatant by adopting a mode of upper water outlet, and removing the supernatant to obtain the residual precipitate which is the phosphorization precipitate: magnesium ammonium phosphate, the recovery of phosphate in this example was determined to be: 51 percent.
Example two:
the difference from the first embodiment is that this embodiment S3 is:
placing the prepared dry sludge in a crucible, placing the crucible in a muffle furnace, setting the temperature to be 900 ℃ for incineration for 2h to obtain sludge incineration ash, cooling the incineration ash to room temperature, placing the sludge incineration ash in a container, and adding 0.2 mol.L-1H of (A) to (B)2SO4Lixiviant at 60mL g-1Under the condition of liquid-solid ratio, the reaction is carried out for 2 hours at normal temperature, then the centrifugal treatment is carried out, sludge supernatant rich in a large amount of phosphorus is obtained, and PO is treated in the supernatant by the embodiment4 3-P concentration was tested and the data were: 38.43mg g-1。
Example three:
the difference from the second embodiment is that this embodiment S3 is:
placing the prepared dry sludge in a crucible, placing the crucible in a muffle furnace, setting the temperature to be 900 ℃ for incineration for 2 hours to obtain sludge incineration ash, cooling the incineration ash to room temperature, placing the sludge incineration ash in a container, and adding 0.6 mol.L-1H of (A) to (B)2SO4Lixiviant at 60mL g-1Under the condition of liquid-solid ratio, the reaction is carried out for 2 hours at normal temperature, then the centrifugal treatment is carried out, sludge supernatant rich in a large amount of phosphorus is obtained, and PO is treated in the supernatant by the embodiment4 3-P concentration was tested and the data were: 42.01mg g-1。
Example four:
the difference from the third embodiment is that this embodiment S3 is:
placing the prepared dry sludge in a crucible, placing the crucible in a muffle furnace, setting the temperature to be 900 ℃ for incineration for 2h to obtain sludge incineration ash, cooling the incineration ash to room temperature, placing the sludge incineration ash in a container, and adding 0.2 mol.L-1H of (A) to (B)2SO4Lixiviant at 60mL g-1Under the condition of liquid-solid ratio, the reaction is carried out for 2 hours at normal temperature, then the centrifugal treatment is carried out, sludge supernatant rich in a large amount of phosphorus is obtained, and PO is treated in the supernatant by the embodiment4 3-P concentration was tested and the data were: 42.07mg g-1Compared with PO in the first embodiment4 3-The leaching amount of-P is increased by 31.4%.
Example five:
the difference from the fourth embodiment is that this embodiment S3 is:
placing the prepared dry sludge in a crucible, placing the crucible in a muffle furnace, setting the temperature to 600 ℃ for incineration for 2h to obtain sludge incineration ash, cooling the incineration ash to room temperature, placing the sludge incineration ash in a container, and adding 0.6 mol.L-1H of (A) to (B)2SO4Lixiviant at 60mL g-1Under the condition of liquid-solid ratio, the reaction is carried out for 2 hours at normal temperature, then the centrifugal treatment is carried out, sludge supernatant rich in a large amount of phosphorus is obtained, and PO is treated in the supernatant by the embodiment4 3-P concentration was tested and the data were: 34.21mg g-1。
Example six:
the difference from the fifth embodiment is that this embodiment S5 is:
s5, taking the supernatant after S4 fine purification as stock solution, putting the stock solution into a container, adjusting the pH value of the stock solution to 8.5, adding MgCl with the ratio of n (Mg) to n (P) being 0.82·6H2O,At 200r/min-1Reacting for 24 hours under stirring, and then reacting at 4000 r.min-1Centrifuging for 10min, removing supernatant to obtain the residual precipitate as phosphorization precipitate, and measuring the recovery rate of phosphate radical in this example as follows: 41 percent.
Example seven:
the sixth difference from the above-mentioned embodiment is that this embodiment S5 is:
s5, taking the supernatant after S4 fine purification as stock solution, putting the stock solution into a container, adjusting the pH value of the stock solution to 9.5, adding MgCl with the ratio of n (Mg) to n (P) being 0.82·6H2O, at 200r/min-1Reacting for 24 hours under stirring, and then reacting at 4000 r.min-1Centrifuging for 10min, removing supernatant to obtain the residual precipitate as phosphorization precipitate, and measuring the recovery rate of phosphate radical in this example as follows: 80 percent.
Example eight:
the seventh difference from the embodiment is that this embodiment S5 is:
s5, taking the supernatant after S4 fine purification as stock solution, putting the stock solution in a container, adjusting the pH value of the stock solution to 11, adding MgCl with the ratio of n (Mg) to n (P) being 0.82·6H2O, at 200r/min-1Reacting for 24 hours under stirring, and then reacting at 4000 r.min-1Centrifuging for 10min, removing supernatant to obtain the residual precipitate as phosphorization precipitate, and measuring the recovery rate of phosphate radical in this example as follows: 78 percent.
Example nine:
the difference from the eighth embodiment is that this embodiment S5 is:
s5, taking the supernatant after S4 fine purification treatment as stock solution, putting the stock solution into a container, adjusting the pH value of the stock solution to 9.5, adding MgCl with the ratio of n (Mg) to n (P) being 1.22·6H2O, at 200r/min-1Reacting for 24 hours under stirring, and then reacting at 4000 r.min-1Centrifuging for 10min, removing supernatant to obtain the residual precipitate as phosphorization precipitate, and measuring the recovery rate of phosphate radical in this example as follows: 88 percent.
Example ten:
the difference from the ninth embodiment is that this embodiment S5 is:
s5, taking the supernatant after S4 fine purification treatment as stock solution, putting the stock solution into a container, adjusting the pH value of the stock solution to 9.5, adding MgCl with the ratio of n (Mg) to n (P) being 1.82·6H2O, at 200r/min-1Reacting for 24 hours under stirring, and then reacting at 4000 r.min-1Centrifuging for 10min, removing supernatant to obtain the residual precipitate as phosphorization precipitate, and measuring the recovery rate of phosphate radical in this example as follows: 86 percent.
From the first to fifth examples, it can be seen that when the incineration temperature is 900 ℃, the TP release rate in the sludge is the largest and gradually increases, and is 0.2 mol. L-1At acid concentration, H2SO4PO in supernatant when used as extractant4 3-The highest concentration of P is 42.07mg g-1。
As can be seen from examples six to eight, when the pH of the solution is in the range of 8.0 to 9.5, the recovery of phosphorus increases with increasing pH; the phosphorus recovery remained essentially unchanged at pH 9.5-11, and was highest at pH 9.5: 80 percent.
From the eighth to tenth examples, it can be seen that MgCl was changed when the pH of the solution was 9.52·6H2The ratio of n (Mg) n (P) of O has an influence on the recovery rate of phosphorus, and when the ratio of n (Mg) n (P) is 1.2, the recovery rate of phosphorus is the highest: 88 percent.
Claims (6)
1. A method for releasing and recovering phosphorus in sludge is characterized by mainly comprising the following steps:
s1, selecting a part of sludge of a sludge treatment plant, adding a flocculating agent into the selected sludge, stirring the sludge added with the flocculating agent to accelerate the flocculation speed, setting the stirring speed to be 200r/min, stirring for 10-25min, performing ultrasonic pretreatment on the stirred sludge, mechanically dehydrating the sludge after the ultrasonic pretreatment, and removing interstitial water and capillary water in the sludge;
s2, drying the dewatered sludge subjected to mechanical dewatering treatment for 12 hours at 105 ℃, removing adsorbed water and water inside the sludge, and grinding the sludge into powder of 100 meshes by a grinder to prepare dry sludge for later use;
s3, placing the prepared dry sludge in a crucible, placing the crucible in a muffle furnace, setting the temperature to 600--1The lixiviant is reacted for 2 hours at normal temperature under the condition of 15-150mL/g liquid-solid ratio and then is centrifugally treated to obtain sludge supernatant rich in a large amount of phosphorus;
s4, adding the obtained sludge supernatant rich in a large amount of phosphorus into a reactor for fine purification: setting pulse voltage of 20Kv and pulse frequency of 200-300Hz, placing the upper and lower electrode plates in the supernatant, and setting the distance between the upper and lower electrode plates to be 8 mm;
s5, taking the supernatant after S4 fine purification as stock solution, putting the stock solution into a container, adjusting the pH value of the stock solution to 8-11, adding MgCl with the ratio of n (Mg) to n (P) of 0.8-22·6H2O, at 200r/min-1Reacting for 24 hours under stirring, and then reacting at 4000 r.min-1Centrifuging for 10min, and removing supernatant to obtain the final product.
2. The method for releasing and recovering phosphorus from sludge as claimed in claim 1, wherein in S3, the residue left after centrifugation is washed with secondary deionized water for several times, returned to the crucible, dried, incinerated and centrifuged.
3. The method for releasing and recovering phosphorus from sludge as claimed in claim 2, wherein the temperature of the residue left after centrifugation in S3 is raised to 1200 ℃ during the second incineration, and after cooling, lixiviant is added, and after 0.5-1h of reaction at normal temperature, the residue is centrifuged to obtain supernatant.
4. The process for the release and recovery of phosphorus from sludge as claimed in claim 1, wherein the leaching agent in S3 is selected from H2SO4HCL and HNO3One of them.
5. The method for releasing and recovering phosphorus from sludge as claimed in claim 1, wherein the supernatant is removed in S5 by discharging the supernatant as a supernatant, and the effluent is covered with a 0.45um filter membrane.
6. The method for releasing and recovering phosphorus from sludge as claimed in claim 1, wherein in S1, the ultrasonic frequency is set to 20-100Hz and the ultrasonic treatment time is set to 10 min.
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CN114933497B (en) * | 2022-06-08 | 2023-02-10 | 四川大学 | Method for preparing N-P compound fertilizer by using excess sludge incineration ash |
CN115159489A (en) * | 2022-07-15 | 2022-10-11 | 华中科技大学 | Method and system for modifying sludge to fix phosphorus and recovering phosphorus based on acid leaching of incineration ash |
CN115159489B (en) * | 2022-07-15 | 2024-06-11 | 华中科技大学 | Method and system for sludge modified phosphorus fixation and phosphorus recovery based on incineration ash acid leaching |
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