CN115400744A - Method for preparing phosphorus adsorbent from sludge ash - Google Patents
Method for preparing phosphorus adsorbent from sludge ash Download PDFInfo
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- CN115400744A CN115400744A CN202211128649.2A CN202211128649A CN115400744A CN 115400744 A CN115400744 A CN 115400744A CN 202211128649 A CN202211128649 A CN 202211128649A CN 115400744 A CN115400744 A CN 115400744A
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- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 title claims abstract description 116
- 239000011574 phosphorus Substances 0.000 title claims abstract description 110
- 229910052698 phosphorus Inorganic materials 0.000 title claims abstract description 110
- 239000010802 sludge Substances 0.000 title claims abstract description 68
- 239000003463 adsorbent Substances 0.000 title claims abstract description 65
- 238000000034 method Methods 0.000 title claims abstract description 47
- 239000011575 calcium Substances 0.000 claims abstract description 46
- 229910052791 calcium Inorganic materials 0.000 claims abstract description 39
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000000654 additive Substances 0.000 claims abstract description 25
- 230000000996 additive effect Effects 0.000 claims abstract description 21
- 239000000203 mixture Substances 0.000 claims abstract description 15
- 239000000126 substance Substances 0.000 claims abstract description 10
- 238000000227 grinding Methods 0.000 claims abstract description 7
- 239000000463 material Substances 0.000 claims abstract description 7
- 238000007873 sieving Methods 0.000 claims abstract description 7
- 238000003760 magnetic stirring Methods 0.000 claims abstract description 5
- 239000011363 dried mixture Substances 0.000 claims abstract description 4
- 239000002985 plastic film Substances 0.000 claims abstract description 4
- 229920006255 plastic film Polymers 0.000 claims abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 26
- 238000001179 sorption measurement Methods 0.000 claims description 22
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 10
- 229910052586 apatite Inorganic materials 0.000 claims description 8
- 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 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 230000035484 reaction time Effects 0.000 claims description 6
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 4
- 210000003278 egg shell Anatomy 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 102000002322 Egg Proteins Human genes 0.000 claims description 2
- 108010000912 Egg Proteins Proteins 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- 239000000243 solution Substances 0.000 description 21
- 239000000047 product Substances 0.000 description 12
- 230000000694 effects Effects 0.000 description 7
- 238000011084 recovery Methods 0.000 description 6
- 229910001385 heavy metal Inorganic materials 0.000 description 5
- 238000005303 weighing Methods 0.000 description 5
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 102000005445 Neuronal Apoptosis-Inhibitory Protein Human genes 0.000 description 2
- 108010006696 Neuronal Apoptosis-Inhibitory Protein Proteins 0.000 description 2
- 238000004220 aggregation Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 238000010790 dilution Methods 0.000 description 2
- 239000012895 dilution Substances 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 239000002910 solid waste Substances 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- 241000192710 Microcystis aeruginosa Species 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011038 discontinuous diafiltration by volume reduction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000012851 eutrophication Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229910000402 monopotassium phosphate Inorganic materials 0.000 description 1
- 235000019796 monopotassium phosphate Nutrition 0.000 description 1
- 235000015097 nutrients Nutrition 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 239000002686 phosphate fertilizer Substances 0.000 description 1
- 239000002367 phosphate rock Substances 0.000 description 1
- PJNZPQUBCPKICU-UHFFFAOYSA-N phosphoric acid;potassium Chemical compound [K].OP(O)(O)=O PJNZPQUBCPKICU-UHFFFAOYSA-N 0.000 description 1
- 239000012254 powdered material Substances 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 239000002918 waste heat Substances 0.000 description 1
- 239000013585 weight reducing agent Substances 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/3078—Thermal treatment, e.g. calcining or pyrolizing
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/3014—Kneading
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/3021—Milling, crushing or grinding
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09B—DISPOSAL OF SOLID WASTE NOT OTHERWISE PROVIDED FOR
- B09B3/00—Destroying solid waste or transforming solid waste into something useful or harmless
- B09B3/30—Destroying solid waste or transforming solid waste into something useful or harmless involving mechanical treatment
- B09B3/35—Shredding, crushing or cutting
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09B—DISPOSAL OF SOLID WASTE NOT OTHERWISE PROVIDED FOR
- B09B3/00—Destroying solid waste or transforming solid waste into something useful or harmless
- B09B3/30—Destroying solid waste or transforming solid waste into something useful or harmless involving mechanical treatment
- B09B3/38—Stirring or kneading
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09B—DISPOSAL OF SOLID WASTE NOT OTHERWISE PROVIDED FOR
- B09B3/00—Destroying solid waste or transforming solid waste into something useful or harmless
- B09B3/40—Destroying solid waste or transforming solid waste into something useful or harmless involving thermal treatment, e.g. evaporation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09B—DISPOSAL OF SOLID WASTE NOT OTHERWISE PROVIDED FOR
- B09B5/00—Operations not covered by a single other subclass or by a single other group in this subclass
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/288—Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4875—Sorbents characterised by the starting material used for their preparation the starting material being a waste, residue or of undefined composition
- B01J2220/4887—Residues, wastes, e.g. garbage, municipal or industrial sludges, compost, animal manure; fly-ashes
-
- 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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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Organic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Water Supply & Treatment (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention discloses a method for preparing a phosphorus adsorbent from sludge ash, which comprises the following steps: a) Putting sludge ash into a beaker, adding a calcium-containing substance in a set proportion as a calcium-based additive to obtain a mixed material, covering the beaker filled with the mixed material with a plastic film, and performing magnetic stirring to uniformly mix the two substances; b) Grinding and sieving the dried mixture, transferring the obtained mixture into a crucible, and placing the crucible into a muffle furnace for co-incineration treatment; c) After the incineration treatment is finished, after the temperature in the muffle furnace is reduced to room temperature, the muffle furnace is opened, the crucible is taken out, the incineration product is ground and sieved to obtain a phosphorus adsorbent, and the phosphorus adsorbent is added into a phosphorus-containing solution to be oscillated to adsorb phosphorus.
Description
Technical Field
The invention relates to the technical field of resource utilization of solid wastes, in particular to a method for preparing a phosphorus adsorbent from sludge ash.
Background
Phosphorus is an indispensable nutrient element for the growth of animals and plants, and plays an important role in agriculture and industrial production. The source of phosphorus in nature is primarily the exploitation of phosphate rock, and it is estimated that new natural phosphate beds will not form worldwide for at least 200 years. Due to the one-way fluidity of phosphorus, more and more phosphorus flows to a water body, thereby causing eutrophication of the water body and causing damages such as water bloom outbreak and the like. Therefore, the focus of current phosphorus resource recovery is on phosphorus recovery from water and phosphorus-containing waste streams. Sludge, a major by-product of municipal sewage treatment, contains more valuable inorganic components and is considered to be the most promising source of phosphorus.
The sludge incineration treatment can completely carbonize organic matters, has better volume reduction and weight reduction effects, and can use waste heat for power generation or heat supply, so the incineration treatment is considered to be the most thorough and rapid method for sludge treatment at present. Sludge ash generated by incineration is P-rich 2 O 5 、SiO 2 、CaO、Al 2 O 3 、Fe 2 O 3 Powdered material of MgO and a large amount of heavy metals, having a high P content 2 O 5 The content, which is usually in the range of 10-25.7%, is of great importance for establishing a process for the recovery of phosphorus from sludge ash. In the prior art, most of the generated sludge incineration ash is subjected to landfill treatment, so that resource waste is generated.
The main method for recovering phosphorus from sludge ash is a thermochemical method, wherein the sludge ash and a calcium-based additive can increase phosphorus bioavailability in the ash and solidify heavy metals through a series of thermochemical reactions at high temperature, however, due to the dilution effect of the calcium-based additive, the phosphorus content of the obtained product is usually low, and therefore, the application of the sludge product prepared by the thermochemical method as a phosphate fertilizer is limited.
In order to solve the problems, the invention provides a phosphorus-containing product prepared from sludge ash and a calcium-based additive as a phosphorus adsorbent, so as to offset the dilution effect of the calcium-based additive on phosphorus in the sludge ash in thermochemical treatment and increase the phosphorus content in the adsorbent, thereby recovering phosphorus in a water body and the sludge ash.
Disclosure of Invention
The invention aims to provide a method for preparing a phosphorus adsorbent by sludge ash so as to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme: a method for preparing a phosphorus adsorbent from sludge ash comprises the following steps:
a) Putting sludge ash into a beaker, adding a calcium-containing substance with a set proportion as a calcium-based additive to obtain a mixed material, covering the beaker filled with the mixed material with a plastic film, performing magnetic stirring to uniformly mix the two substances, stirring for at least 1h, and putting the uniformly mixed mixture into an oven for drying;
b) Grinding and sieving the dried mixture, transferring the obtained mixture into a crucible, placing the crucible in a muffle furnace, carrying out co-incineration treatment, controlling the incineration conditions of the mixed sample by setting the parameters of the muffle furnace, and adding a small amount of deionized water in the incineration process;
c) After the incineration treatment is finished, after the temperature in the muffle furnace is reduced to room temperature, the muffle furnace is opened, the crucible is taken out, the incineration product is ground and sieved to obtain a phosphorus adsorbent, the phosphorus adsorbent is added into a phosphorus-containing solution to be vibrated so as to adsorb phosphorus, and after the adsorption is finished, solid and liquid are separated, and solid matters are dried.
Preferably, the method for preparing the phosphorus adsorbent from the sludge ash is provided, wherein calcium carbonate, eggshell and shell calcium carbonate-containing substances are adopted as the calcium-based additive in the step A).
Preferably, the method for preparing the phosphorus adsorbent from the sludge ash is provided by the application, wherein in the step A), the mass ratio of the sludge ash to the calcium-based additive is 5:1 to 1:1, were mixed.
Preferably, the application provides a method for preparing the phosphorus adsorbent from sludge ash, wherein in the step A), the uniformly mixed mixture is placed into an oven and is dried for no more than 12 hours at the temperature of no higher than 105 ℃.
Preferably, the method for preparing the phosphorus adsorbent from the sludge ash is provided, wherein in the step B), the incineration temperature is set to be not lower than 750 ℃ and the reaction time is set to be at least 1h in the co-incineration treatment process.
Preferably, the application provides a method for preparing the phosphorus adsorbent by using sludge ash, wherein in the step C), in the incineration product, the content of non-apatite inorganic phosphorus is not more than 5% of total phosphorus; the conversion rate of non-apatite inorganic phosphorus to apatite state phosphorus is not less than 95%.
Preferably, in the step C), the incineration product is ground and sieved by a 100-mesh sieve, and then placed in a vacuum drier for storage.
Preferably, in the step C), the adding amount ratio of phosphorus in the phosphorus-containing solution to the adsorbent is 10-150 mg phosphorus/g adsorbent, and the reaction time of the adsorbent and the phosphorus-containing solution is not less than 6 hours.
Preferably, the application provides a method for preparing a phosphorus adsorbent from sludge ash, wherein in the step C), the adsorbed adsorbent is dried in an oven at a temperature of not higher than 105 ℃; the phosphorus content in the adsorbed adsorbent is higher than that of original sludge ash; the content of non-apatite inorganic phosphorus in the adsorbent after adsorption is not higher than 10% of the total phosphorus.
Compared with the prior art, the invention has the beneficial effects that:
(1) The invention selects calcium-containing substances as exogenous calcium-based additives to be co-burned with sludge ash, aiming at obtaining phosphorus-containing products with high bioavailability form phosphorus and low heavy metal content; by controlling the adding proportion of the sludge ash and the calcium-based additive, the maximum conversion from the phosphorus form with low bioavailability to the phosphorus form with high bioavailability is realized, and a foundation is laid for recovering phosphorus in the sludge ash to the maximum extent;
(2) The method of the invention uses the adsorbent prepared from the sludge ash to adsorb phosphorus in the water body, thereby realizing the recovery and aggregation of phosphorus elements in the water body and the sludge ash;
(3) The adsorbent prepared by the invention is rich in a large amount of phosphorus elements after phosphorus adsorption, even exceeds sludge ash, can make a great contribution to relieving the problem of phosphorus resource shortage, and simultaneously realizes the recycling and reduction of the sludge ash.
Drawings
FIG. 1 is a graph showing the phosphorus content and morphology of the adsorbent and the adsorbent prepared in example 1 after adsorption;
FIG. 2 is a graph showing the effect of the addition of the adsorbent prepared in example 1 on the adsorption of phosphorus in a water body;
FIG. 3 is a graph showing the effect of the adsorbents prepared in example 1 on the adsorption of phosphorus in a water body at different pH values;
FIG. 4 is a graph showing S-Ca adsorption kinetics of phosphorus by the adsorbent prepared in example 1;
FIG. 5 is a graph showing S-ES adsorption kinetics of phosphorus adsorption by the adsorbent prepared in example 1;
FIG. 6 is a S-Ca adsorption isotherm plot of phosphorus adsorbed by the adsorbent prepared in example 1;
FIG. 7 is a S-ES adsorption isotherm plot of phosphorus adsorption by the adsorbent prepared in example 1;
FIG. 8 is a schematic of the phosphorus removal rate of the adsorbent prepared in example 1 adsorbing phosphorus.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.
The first embodiment is as follows:
a method for preparing a phosphorus adsorbent from sludge ash comprises the following steps:
a) Weighing 10g of sludge ash, placing the sludge ash in a beaker, respectively adding calcium carbonate and egg shells serving as calcium-based additives, wherein the weights of the calcium-based additives are 1g, 2g and 3g respectively, adding a small amount of deionized water, then covering the beaker filled with the mixed material by using a plastic film, performing magnetic stirring to uniformly mix the sludge ash and the calcium-based additives, stirring for 1h, placing the uniformly mixed mixture in an oven, and drying for 12h at 105 ℃;
b) Grinding the dried mixture, sieving the ground mixture by a 100-mesh sieve, transferring the obtained mixture into a crucible, placing the crucible into a muffle furnace, carrying out co-incineration treatment, incinerating the mixture for 2 hours at 850 ℃, and adding a small amount of deionized water in the incineration process;
c) After the incineration treatment is finished, after the temperature in the muffle furnace is reduced to room temperature, opening the muffle furnace, taking out the crucible, grinding the incineration product, sieving the incineration product by a 100-mesh sieve, and storing the incineration product in a vacuum drier;
d) Weighing 0.16g of the adsorbent prepared in the step C), adding the adsorbent into 30mL100 mg/L of solution containing P, putting the solution into a shaking table, oscillating for 24h, drying at 105 ℃ for 12h after the reaction is finished, grinding the adsorbent after the adsorption is finished, sieving by a 100-mesh sieve, and putting the adsorbent into a vacuum drier for storage.
Through detection, the total phosphorus and NAIP content of the sludge ash and the calcium-based additive are reduced after the sludge ash and the calcium-based additive are incinerated together, the AP content is increased, as shown in figure 1, when the calcium-based additive content is 3g, namely 30% of the calcium-based additive dosage, the NAIP basically disappears and is converted into AP, the calcium-based additive prepared by 30% of the dosage is selected as the optimal adsorbent (S-Ca and S-ES), and the phosphorus content of the adsorbent is increased after the adsorption is finished, even higher than the phosphorus content of the original sludge ash and the like.
Example two:
the method for researching the influence of the addition amount of the adsorbent on phosphorus adsorption comprises the following steps:
a) Preparing 100mg/L solution containing P, and placing 30mL of solution into a centrifuge tube;
b) 0.01g, 0.02g, 0.04g, 0.08g, 0.16g, 0.24g, 0.32g and 0.40g of S-Ca and S-ES prepared in example 1 are weighed and added into a) centrifuge tube, and three parallel samples are arranged at each adding amount;
c) The centrifuge tube was placed in a shaker and shaken for 24h.
As shown in FIG. 2, phosphorus removal rates in the solutions were as high as 97.91% and 100% for S-Ca and S-ES.
The third embodiment of the present invention is detailed as follows:
a) Preparing 100mg/L solution containing P, and adjusting the pH value by using NaOH and HCl solution with negligible volume, wherein the pH value ranges from 2 to 12;
b) Respectively weighing 0.16g of S-Ca and S-ES prepared in the embodiment 1, adding the S-Ca and the S-ES into a centrifuge tube, and setting three parallel samples under different pH conditions;
c) Adding 30mL of the solution prepared in the step A) into a centrifuge tube of the step B), placing the centrifuge tube into a shaking table, and shaking for 24 hours.
As is clear from FIG. 3, the adsorbents prepared in this example all have a good effect of adsorbing phosphorus at pH 4 to 12, except under strongly acidic conditions (pH 2).
Example four of the present invention is detailed as follows:
a) Preparing 100mg P/L solution, sucking 30mL of solution and placing the solution in a centrifuge tube;
b) Weighing 0.16g of S-Ca and S-ES prepared in the example 1, adding the S-Ca and the S-ES into a centrifuge tube, and setting three parallel samples under different reaction time conditions;
c) Placing the centrifuge tube into shaking table, and shaking for 10min, 30min, 60min, 120min, 180min, 360min, 720min and 1440min.
The experimental results were fitted using the pseudo first order kinetic equation and the pseudo second order kinetic equation, and the fitting results are shown in fig. 4 and 5, where the adsorption process of S-Ca more conforms to the pseudo second order kinetic equation, and the adsorption process of S-ES more conforms to the pseudo first order kinetic equation.
Example five of the present invention is detailed as follows:
a) Preparing solutions containing P at 50mg/L, 100mg/L, 150mg/L, 200mg/L, 300mg/L and 600mg/L, sucking 30mL of the prepared solution and placing the solution in a centrifuge tube;
b) Weighing 0.16g of S-Ca and S-ES prepared in the example 1, adding the S-Ca and the S-ES into a centrifuge tube, and setting three parallel samples under different reaction time conditions;
c) The centrifuge tube was placed in a shaker for 24h of shaking time.
Adsorption isotherm data fitting was performed using Langmuir and Freundlich models, and the fitting results are shown in fig. 6 and 7, which resulted in the fitting adsorption isotherms of both S-Ca and S-ES more conforming to the Freundlich models.
Example six of the present invention is detailed as follows:
a) Taking 30mL of actual river water, adding potassium dihydrogen phosphate until the content of P is 10mg/L, and preparing 10mg/L of solution containing P by using deionized water;
b) 0.01g, 0.02g, 0.04g, 0.08g, 0.16g, 0.24g, 0.32g and 0.40g of the S-Ca and the S-ES prepared in the example 1 are weighed and added into a P-containing solution prepared by A) river water containing P and deionized water, and three parallel samples are arranged under the condition of different adding amounts;
c) The centrifuge tube was placed in a shaker for 24h of shaking time.
As can be seen from FIG. 8, the S-Ca and S-ES prepared by the invention have good removing capability to phosphorus in river water, and when the adding amount is 0.04g, phosphorus in river water is basically removed; compared with the solution containing P prepared by deionized water, S-Ca and S-ES have slightly poor effect on removing phosphorus in river water, but the maximum difference is only within 6 percent.
The embodiment relates to an adsorbent prepared from sludge ash to recover phosphorus in water and sludge, and is applied to the technical field of resource utilization of solid wastes. The method of the embodiment mixes the sludge ash and the calcium-based additive in a certain proportion, uniformly mixes the sludge ash and the calcium-based additive in a magnetic stirring mode, and prepares the adsorbent in a co-incineration mode to adsorb phosphorus in the water body, so as to enrich and recover the phosphorus in the water body and the sludge. The method of the embodiment can realize the high-efficiency recovery of the sludge incineration ash and phosphorus resources in the water body and the reduction of the sludge ash, and meanwhile, the content of heavy metals in the obtained phosphorus-containing product is far lower than the specified limit value, so that the method has a good industrial application prospect.
In conclusion, the invention selects the calcium-containing substance as the exogenous calcium-based additive to be co-incinerated with the sludge ash, aiming at obtaining the phosphorus-containing product with high bioavailability shape phosphorus and low heavy metal content; by controlling the adding proportion of the sludge ash and the calcium-based additive, the maximum conversion from the phosphorus form with low bioavailability to the phosphorus form with high bioavailability is realized, and a foundation is laid for recovering phosphorus in the sludge ash to the maximum extent; the method of the invention uses the adsorbent prepared from the sludge ash to adsorb the phosphorus in the water body, thereby realizing the recovery and aggregation of phosphorus elements in the water body and the sludge ash; the adsorbent prepared by the invention is rich in a large amount of phosphorus elements after phosphorus adsorption, even exceeds sludge ash, can make a great contribution to relieving the problem of phosphorus resource shortage, and simultaneously realizes the recycling and reduction of the sludge ash.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Claims (9)
1. A method for preparing a phosphorus adsorbent from sludge ash is characterized by comprising the following steps: the method comprises the following steps:
a) Putting sludge ash into a beaker, adding a calcium-containing substance with a set proportion as a calcium-based additive to obtain a mixed material, covering the beaker filled with the mixed material with a plastic film, performing magnetic stirring to uniformly mix the two substances, stirring for at least 1h, putting the uniformly mixed mixture into an oven, and drying;
b) Grinding and sieving the dried mixture, transferring the obtained mixture into a crucible, placing the crucible in a muffle furnace, carrying out co-incineration treatment, controlling the incineration conditions of the mixed sample by setting the parameters of the muffle furnace, and adding a small amount of deionized water in the incineration process;
c) After the incineration treatment is finished, after the temperature in the muffle furnace is reduced to room temperature, the muffle furnace is opened, the crucible is taken out, the incineration product is ground and sieved to obtain a phosphorus adsorbent, the phosphorus adsorbent is added into a phosphorus-containing solution to be oscillated to adsorb phosphorus, and after the adsorption is finished, solid and liquid are separated, and solid matters are dried.
2. The method for preparing the phosphorus adsorbent by using the sludge ash as claimed in claim 1, wherein the method comprises the following steps: the calcium-based additive in the step A) adopts calcium carbonate, eggshell and shell calcium carbonate-containing substances.
3. The method for preparing the phosphorus adsorbent from the sludge ash as claimed in claim 1, is characterized in that: in the step A), the sludge ash and the calcium-based additive are mixed according to the mass ratio of 5:1 to 1:1, were mixed.
4. The method for preparing the phosphorus adsorbent by using the sludge ash as claimed in claim 1, wherein the method comprises the following steps: in the step A), the uniformly mixed mixture is put into an oven and is dried for no more than 12 hours at the temperature of no more than 105 ℃.
5. The method for preparing the phosphorus adsorbent by using the sludge ash as claimed in claim 1, wherein the method comprises the following steps: in the step B), in the co-incineration treatment process, the incineration temperature is set to be not lower than 750 ℃, and the reaction time is at least 1h.
6. The method for preparing the phosphorus adsorbent from the sludge ash as claimed in claim 1, is characterized in that: in the step C), the content of non-apatite inorganic phosphorus in the incineration product is not more than 5 percent of total phosphorus; the conversion rate of the non-apatite inorganic phosphor to apatite phosphor is not less than 95%.
7. The method for preparing the phosphorus adsorbent by using the sludge ash as claimed in claim 1, wherein the method comprises the following steps: and in the step C), grinding the incineration product, sieving the incineration product by a 100-mesh sieve, and storing the incineration product in a vacuum drier.
8. The method for preparing the phosphorus adsorbent by using the sludge ash as claimed in claim 1, wherein the method comprises the following steps: in the step C), the adding amount ratio of phosphorus in the phosphorus-containing solution to the adsorbent is 10-150 mg of phosphorus/g of adsorbent, and the reaction time of the adsorbent and the phosphorus-containing solution is not less than 6 hours.
9. The method for preparing the phosphorus adsorbent by using the sludge ash as claimed in claim 1, wherein the method comprises the following steps: in the step C), drying the adsorbed adsorbent in an oven at a temperature of not higher than 105 ℃; the phosphorus content in the adsorbed adsorbent is higher than that of original sludge ash; the content of non-apatite inorganic phosphorus in the adsorbent after adsorption is not higher than 10% of total phosphorus.
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