CN115815317A - Method for recycling sludge and preparing soil conditioner - Google Patents
Method for recycling sludge and preparing soil conditioner Download PDFInfo
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- CN115815317A CN115815317A CN202211611943.9A CN202211611943A CN115815317A CN 115815317 A CN115815317 A CN 115815317A CN 202211611943 A CN202211611943 A CN 202211611943A CN 115815317 A CN115815317 A CN 115815317A
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- hydrothermal
- leaching
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- sludge
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- 239000010802 sludge Substances 0.000 title claims abstract description 40
- 238000000034 method Methods 0.000 title claims abstract description 25
- 239000003516 soil conditioner Substances 0.000 title claims abstract description 13
- 238000004064 recycling Methods 0.000 title abstract description 6
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims abstract description 34
- 229910052698 phosphorus Inorganic materials 0.000 claims abstract description 34
- 239000011574 phosphorus Substances 0.000 claims abstract description 34
- 238000002386 leaching Methods 0.000 claims abstract description 27
- 238000006243 chemical reaction Methods 0.000 claims abstract description 19
- 210000003278 egg shell Anatomy 0.000 claims abstract description 17
- 238000003763 carbonization Methods 0.000 claims abstract description 15
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 14
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 claims abstract description 14
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 13
- 239000002296 pyrolytic carbon Substances 0.000 claims abstract description 13
- 239000002253 acid Substances 0.000 claims abstract description 11
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 10
- 235000021110 pickles Nutrition 0.000 claims abstract description 10
- 238000003756 stirring Methods 0.000 claims abstract description 9
- 102000002322 Egg Proteins Human genes 0.000 claims abstract description 8
- 108010000912 Egg Proteins Proteins 0.000 claims abstract description 8
- 239000007788 liquid Substances 0.000 claims abstract description 7
- 229910001629 magnesium chloride Inorganic materials 0.000 claims abstract description 7
- 239000010902 straw Substances 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000008367 deionised water Substances 0.000 claims abstract description 6
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 6
- 239000000203 mixture Substances 0.000 claims abstract description 6
- 238000001914 filtration Methods 0.000 claims abstract description 4
- 238000002156 mixing Methods 0.000 claims abstract description 4
- 238000000197 pyrolysis Methods 0.000 claims abstract description 4
- 238000000926 separation method Methods 0.000 claims abstract description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 3
- 238000002791 soaking Methods 0.000 claims abstract description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract 4
- 238000011049 filling Methods 0.000 claims abstract 2
- 230000008569 process Effects 0.000 claims description 7
- 239000000654 additive Substances 0.000 claims description 6
- 239000011083 cement mortar Substances 0.000 claims description 6
- 230000000996 additive effect Effects 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 3
- 238000005119 centrifugation Methods 0.000 claims description 2
- 239000003610 charcoal Substances 0.000 claims 1
- 229910001385 heavy metal Inorganic materials 0.000 description 13
- 238000001179 sorption measurement Methods 0.000 description 5
- 238000011084 recovery Methods 0.000 description 4
- 229910052586 apatite Inorganic materials 0.000 description 3
- 230000008878 coupling Effects 0.000 description 3
- 238000010168 coupling process Methods 0.000 description 3
- 238000005859 coupling reaction Methods 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- VSIIXMUUUJUKCM-UHFFFAOYSA-D pentacalcium;fluoride;triphosphate Chemical compound [F-].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O VSIIXMUUUJUKCM-UHFFFAOYSA-D 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 244000005700 microbiome Species 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 239000002689 soil Substances 0.000 description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 239000002154 agricultural waste Substances 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 238000005341 cation exchange Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000003337 fertilizer Substances 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 239000003546 flue gas Substances 0.000 description 1
- 238000002309 gasification Methods 0.000 description 1
- 231100001261 hazardous Toxicity 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 239000002910 solid waste Substances 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000004083 survival effect Effects 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 238000007704 wet chemistry method Methods 0.000 description 1
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/40—Valorisation of by-products of wastewater, sewage or sludge processing
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- Processing Of Solid Wastes (AREA)
Abstract
The invention discloses a method for recycling sludge and preparing a soil conditioner, which comprises the following steps: filling nitrogen into the hydrothermal reaction kettle to discharge air, feeding sludge into the reaction kettle to perform hydrothermal carbonization reaction, and performing solid-liquid separation on the obtained hydrothermal product after the reaction is finished to obtain hydrothermal carbon; mixing hydrothermal carbon and eggshell, placing the mixture in an incinerator, introducing air, incinerating to obtain incineration ash, adding deionized water into the incineration ash, then adding concentrated sulfuric acid, adjusting pH, stirring for phosphorus leaching, intermittently adding concentrated sulfuric acid during leaching to keep the pH stable, and after leaching is finished, performing centrifugal filtration to respectively obtain acid leaching solution and acid leaching residue; soaking the straws and the eggshells into a magnesium chloride solution, modifying the straws and the eggshells by magnesium chloride, and then carrying out high-temperature pyrolysis to obtain pyrolytic carbon; the pyrolytic carbon adsorbs phosphorus in the pickle liquor, and the obtained phosphorus-rich biochar can be directly used as a soil conditioner.
Description
Technical Field
The invention belongs to the technical field of sludge treatment and recycling, and particularly relates to a method for sludge recycling and soil conditioner preparation.
Background
The sludge disposal and resource utilization approaches include landfill, incineration, pyrolysis, gasification and the like, and incineration is a preferable means for treating sludge. However, the hazardous compounds contained in the sludge result in a higher content of flue gas pollutants in the ordinary incineration process. In addition, in the recovery process of phosphorus in the sludge incineration ash, more impurity ions and heavy metals increase purification steps, and the phosphorus recovery difficulty is improved. Therefore, the problems to be solved at present are to improve the cleaning degree of the sludge and to realize the efficient recovery and utilization of phosphorus in the sludge.
The recovery of phosphorus in the sludge incineration ash is usually carried out by adopting a thermochemical method and a wet-chemical method, but the thermochemical method has high energy consumption, complex operation and high cost; wet chemistry methods are distinguished according to the characteristics of ash, heavy metal effects need to be considered heavily, and phosphorus products are often not highly pure. In the hydrothermal carbonization process of the sludge, the forms of heavy metals can be changed to more stable oxidizable states and residue states, and the heavy metals in the hydrothermal carbon have better stability.
The biochar has a highly enriched carbon skeleton and a loose porous structure on the surface, can enhance the water and fertilizer retention capacity of soil, provides survival space for microorganisms when applied to the soil, and promotes the propagation and increment of the microorganisms. In addition, the biochar also has stronger adsorption capacity and higher cation exchange capacity, and a small part of movable compounds.
Disclosure of Invention
In view of the above problems, the present invention aims to provide a method for resource utilization of sludge and preparation of soil conditioner. The sludge is treated by adopting a hydrothermal carbonization coupling incineration mode, so that the purposes of degrading organic matters, removing most of N, S and other pollution elements, enriching phosphorus in sludge ash and stabilizing heavy metals are achieved; adopting agricultural waste modified pyrolytic carbon as an adsorbent to adsorb phosphorus in sludge incineration ash pickle liquor, and taking the obtained phosphorus-rich biochar as a soil conditioner; the residue of the pickle liquor is used as a cement mortar additive. On the one hand, the problem that the smoke pollutants are more in the incineration process of the sludge is solved, on the other hand, the phosphorus in the sludge incineration ash can be simply and efficiently utilized, and the sludge incineration ash can be utilized in multiple ways.
In order to achieve the purpose, the following technical scheme is provided:
(1) Hydrothermal carbonization treatment: and (3) conveying the sludge into a hydrothermal reaction kettle for hydrothermal carbonization reaction, wherein the solid-liquid ratio is preferably 1: (10-20), before hydrothermal carbonization reaction, N is filled into the reaction kettle 2 Discharging air, preferably selecting the stirring speed of the hydrothermal reaction kettle to be 250-350r/min, carrying out hydrothermal carbonization reaction at a set temperature, preferably selecting the temperature to be 210-280 ℃, preferably selecting the hydrothermal reaction time to be 2-4h, and carrying out solid-liquid separation on a hydrothermal product obtained after the reaction is finished.
(2) Incineration treatment: and burning the hydrothermal carbon obtained by hydrothermal carbonization, wherein the burned hydrothermal carbon is mixed with eggshells, and the proportion of the mixed eggshells is preferably 6-12 wt%. And (3) placing the mixture into an incinerator, introducing air, setting the incinerator temperature, preferably 800-900 ℃, and preferably 1-2h for incineration. The hydrothermal carbon is mixed with the eggshell for incineration, the biological availability of phosphorus in the obtained incineration ash is higher, the stable state of heavy metal is greatly increased, and most of the eggshell is made of CaCO 3 The composition is changed into CaO in the incineration process, the CaO promotes the conversion of the phosphorus in the sludge from non-apatite inorganic phosphorus to apatite inorganic phosphorus, and the apatite inorganic phosphorus has better bioavailability, so that the bioavailability of the phosphorus in the incineration ash is improved. In the hydrothermal process of the sludge, the form of the heavy metal can be converted to a more stable oxidizable state and a residue state, the heavy metal in the hydrothermal carbon has better stability, and the conversion of the heavy metal to the stable state can be further promoted in the incineration process of adding CaO. The hydrothermal coupling incineration and the addition of CaO have positive effects on reducing the ecological risk of the sludge ash.
(3) Leaching phosphorus: h for sludge hydrothermal carbon incineration ash 2 SO 4 Leaching, adding incineration ash into deionized water, and then adding concentrated H 2 SO 4 The pH is adjusted, preferably to 1-2. Thereafter concentrated H is added intermittently 2 SO 4 To keep the pH stable, the leaching time is preferably 6-12 hours, and the stirring is continued, and the rotating speed is 150-250r/min. After the leaching is finished, the acid leaching solution and the acid leaching residue are respectively obtained through centrifugation and filtration, wherein the centrifugal rotation speed is preferably 8000 r/min-12000 r/min, and the time is preferably 8-15min.
(4) Acid leaching residue treatment: the acid-leached residues can be used for cement mortar additives, and high phosphorus content is considered as a negative factor of using sludge ash for cement mortar additives, but the acid-leached residues have low phosphorus content and less influence on mechanical strength, so the residues have better mechanical strength.
(5) Preparing modified pyrolytic carbon: the straws and the eggshells are immersed in a magnesium chloride solution, modified by magnesium chloride and then pyrolyzed at high temperature to obtain the pyrolytic carbon with good adsorption performance.
(6) Adsorption of pyrolytic carbon on phosphorus in pickle liquor: the phosphorus in the pickle liquor is absorbed by the modified pyrolytic carbon, and because heavy metal in the ash exists in a stable state after hydrothermal carbonization and mixed eggshell firing, the heavy metal and some impurity ions are less leached during acid leaching. The obtained phosphorus-rich biochar can be directly used for a soil conditioner.
Compared with the prior art, the invention has the beneficial effects that:
1) Sludge is treated by a hydrothermal carbonization coupling incineration mode to prepare sludge ash rich in phosphorus and stable in heavy metal, so that the bioavailability of phosphorus in the sludge is improved, and the leachability of heavy metal in the sludge ash is reduced.
2) The straw and eggshell modified pyrolytic biochar have the advantage of good adsorption property, phosphorus in sludge incineration ash leaching solution is recycled, a soil conditioner is prepared, leaching residues are used as cement mortar additives, solid waste combination and multiple utilization are realized, sludge reduction and harmless treatment are realized, and waste is recycled.
Drawings
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
The technical method in the embodiments of the present invention is clearly and completely described below.
As shown in figure 1, the method for recycling sludge and preparing the soil conditioner comprises the following steps:
hydrothermal carbonization treatment: the sludge is subjected to hydrothermal reaction in a mode of mixing dry sludge and deionized water, and the solid-liquid ratio is set to be 1:10; hydrothermal carbonization reactionBefore, N is filled into the reaction kettle 2 Discharging air, setting the stirring speed of the hydrothermal reaction kettle to be 300r/min, carrying out hydrothermal carbonization reaction at a set temperature of 240 ℃, setting the hydrothermal reaction time to be 4h, and carrying out solid-liquid separation on a hydrothermal product obtained after the reaction is finished.
Incineration treatment: the hydrothermal carbon obtained by hydrothermal carbonization is dried, crushed and mixed with the eggshell powder, and the mixing proportion is 10wt%. And (3) putting the mixture into an incinerator, introducing air, setting the temperature of the incinerator to 850 ℃, setting the incineration time to 1h, and incinerating the eggshell mixed with the hydrothermal carbon.
Leaching phosphorus: h for sludge hydrothermal carbon incineration ash 2 SO 4 Leaching, adding ash into deionized water, and adding concentrated H 2 SO 4 Adjusting the pH, setting the pH to 2, after which concentrated H is added intermittently 2 SO 4 To keep the PH stable, the leaching time was set at 12 hours. Continuously stirring at the rotating speed of 250r/min, centrifuging for 15min at 8000r/min after the reaction is finished, and filtering with a 0.45mm filter membrane to obtain pickle liquor and pickle residues.
Preparing modified pyrolytic carbon: soaking the straws and the eggshells into the magnesium chloride solution, continuously stirring for 6 hours, then placing the mixture in a drying box for drying, and then washing the high-temperature pyrolysis pyrolytic carbon with deionized water and drying for later use.
Adsorption of pyrolytic carbon on phosphorus in pickle liquor: the modified pyrolytic carbon is used for adsorbing phosphorus in the pickle liquor, and the obtained phosphorus-rich biochar can be directly used for a soil conditioner.
Acid leaching residue treatment: the acid leaching residue can be used for cement mortar additive after being filtered.
Claims (8)
1. A method for resource utilization of sludge and preparation of soil conditioner is characterized by comprising the following steps:
1) Filling nitrogen into the reaction kettle to discharge air, feeding sludge into the reaction kettle to perform hydrothermal carbonization reaction, and after the reaction is finished, performing solid-liquid separation on the obtained hydrothermal product to obtain hydrothermal carbon;
2) Mixing the hydrothermal carbon obtained in the step 1) with eggshells, placing the mixture in an incinerator, introducing air, and incinerating to obtain incineration ash;
3) Adding deionized water into the incineration ash obtained in the step 2), then adding concentrated sulfuric acid, adjusting the pH value, stirring for phosphorus leaching, intermittently adding concentrated sulfuric acid in the leaching process to keep the pH value stable, and after leaching is finished, respectively obtaining acid leaching solution and acid leaching residue through centrifugal filtration, wherein the acid leaching residue is used as a cement mortar additive;
4) Soaking the straws and the eggshells into a magnesium chloride solution, modifying the straws and the eggshells by magnesium chloride, and then carrying out high-temperature pyrolysis to obtain pyrolytic carbon;
5) Adsorbing phosphorus in the pickle liquor in the step 3) by using the pyrolytic carbon in the step 4) to obtain phosphorus-rich biochar which can be directly used as a soil conditioner.
2. The method as claimed in claim 1, wherein the solid-to-liquid ratio of the sludge in step 1) is 1.
3. The method according to claim 1, wherein the hydrothermal reaction temperature in step 1) is 210-280 ℃, the hydrothermal reaction time is 2-4h, and the stirring speed of the reaction kettle is 250-350r/min.
4. The method of claim 1, wherein the eggshell is added to the hydrothermal charcoal in the step 2) at a ratio of 6wt% to 12wt%.
5. The method of claim 1, wherein the incineration in step 2) is carried out at a temperature of 800-900 ℃ for a time of 1-2h.
6. The method of claim 1, wherein concentrated sulfuric acid is added in step 3) to adjust the pH to 1-2.
7. The method as claimed in claim 1, wherein the stirring speed in step 3) is 150-250r/min and the leaching time is 6-12h.
8. The method as set forth in claim 1, wherein the centrifugation in step 3) is carried out at a rotation speed of 8000 to 12000r/min for 8 to 15min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211611943.9A CN115815317A (en) | 2022-12-15 | 2022-12-15 | Method for recycling sludge and preparing soil conditioner |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211611943.9A CN115815317A (en) | 2022-12-15 | 2022-12-15 | Method for recycling sludge and preparing soil conditioner |
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| Publication Number | Publication Date |
|---|---|
| CN115815317A true CN115815317A (en) | 2023-03-21 |
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| CN202211611943.9A Pending CN115815317A (en) | 2022-12-15 | 2022-12-15 | Method for recycling sludge and preparing soil conditioner |
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Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4287069A (en) * | 1979-05-21 | 1981-09-01 | Bayer Aktiengesellschaft | Process for the improved working up of effluent |
| US6022514A (en) * | 1998-05-18 | 2000-02-08 | Nkk Corporation | Method for recovering phosphorus from organic sludge |
| JP2008000707A (en) * | 2006-06-23 | 2008-01-10 | Natoo Kenkyusho:Kk | Method of reforming phosphorus-containing burned ash and pollution-free phosphorus-containing recycle material |
| EP3305724A1 (en) * | 2016-10-04 | 2018-04-11 | Hochschule Merseburg | Method for the recovery of phosphorus |
| CN112191229A (en) * | 2020-10-19 | 2021-01-08 | 农业农村部环境保护科研监测所 | Preparation method and application of Mg/Ca-loaded modified tobacco stalk biochar |
| CN113072267A (en) * | 2021-03-05 | 2021-07-06 | 华中科技大学 | Method for efficiently recovering phosphorus from municipal sludge and synchronously preparing porous biochar |
| CN113277690A (en) * | 2021-05-12 | 2021-08-20 | 华中科技大学 | Method and product for comprehensive treatment of sludge and recovery of phosphorus resources |
| 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 |
-
2022
- 2022-12-15 CN CN202211611943.9A patent/CN115815317A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4287069A (en) * | 1979-05-21 | 1981-09-01 | Bayer Aktiengesellschaft | Process for the improved working up of effluent |
| US6022514A (en) * | 1998-05-18 | 2000-02-08 | Nkk Corporation | Method for recovering phosphorus from organic sludge |
| JP2008000707A (en) * | 2006-06-23 | 2008-01-10 | Natoo Kenkyusho:Kk | Method of reforming phosphorus-containing burned ash and pollution-free phosphorus-containing recycle material |
| EP3305724A1 (en) * | 2016-10-04 | 2018-04-11 | Hochschule Merseburg | Method for the recovery of phosphorus |
| CN112191229A (en) * | 2020-10-19 | 2021-01-08 | 农业农村部环境保护科研监测所 | Preparation method and application of Mg/Ca-loaded modified tobacco stalk biochar |
| CN113072267A (en) * | 2021-03-05 | 2021-07-06 | 华中科技大学 | Method for efficiently recovering phosphorus from municipal sludge and synchronously preparing porous biochar |
| CN113277690A (en) * | 2021-05-12 | 2021-08-20 | 华中科技大学 | Method and product for comprehensive treatment of sludge and recovery of phosphorus resources |
| 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 |
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